CN102558677A - Novel scratch-resistant polypropylene composite material and preparation method thereof - Google Patents
Novel scratch-resistant polypropylene composite material and preparation method thereof Download PDFInfo
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- CN102558677A CN102558677A CN2011104421260A CN201110442126A CN102558677A CN 102558677 A CN102558677 A CN 102558677A CN 2011104421260 A CN2011104421260 A CN 2011104421260A CN 201110442126 A CN201110442126 A CN 201110442126A CN 102558677 A CN102558677 A CN 102558677A
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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
- B29C48/03—Extrusion 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
- B29C48/04—Particle-shaped
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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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means 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
- B29C48/40—Means 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
-
- 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
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
-
- 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
-
- 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
- B29C2948/92514—Pressure
-
- 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
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
-
- 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
- B29C2948/92704—Temperature
-
- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a novel scratch-resistant polypropylene composite material and a preparation method thereof. The novel scratch-resistant polypropylene composite material comprises raw materials with the weight percentages as follows: 58 to 98 percent of polypropylene, 0 to 25 percent of inorganic filler, 0 to 15 percent of toughening agent POEO, 0.5 to 4 percent of fluorinated organosilicon, 0.1 to 1 percent of antioxidant, 0.1 to 1 percent of light stabilizer and 0 to 3 percent of other additives. The preparation method of the novel scratch-resistant polypropylene composite material comprises the steps that the raw materials are weighed according to a weight ratio; then the polypropylene, the inorganic filler, the toughening agent, the fluorinated organosilicon, the antioxidant, the light stabilizer and the other additives are mixed in a high speed agitator and then put into a twin-screw extruder to be melted and extruded; and after being extruded, an obtained mixture is cooled, dried and granulated and then a finished product is obtained. The preparation method has the advantages that the fluorinated organosilicon additive is added to a basic formula of the polypropylene material, so that the polypropylene composite material with excellent scratch-resistant performance is prepared; and meanwhile, the polypropylene composite material has good mechanical performance and good wear resistant performance.
Description
Technical field
The present invention relates to a kind of novel scratch-proof polypropylene matrix material and preparation method thereof, can be used for automotive trim, belong to polymer modification and processing technique field.
Background technology
Vestolen PP 7052 has good processing properties and physics, mechanics, chemical property, simultaneously light weight, inexpensive thereby be widely used in inner and outer decorative parts of automobile.But the mar-proof performance of Vestolen PP 7052 is relatively poor, when being applied to test board, automotive trim such as door inner panel etc., directly influences the attractive in appearance of automobile because of the surface is easy to the scuffing meeting, and this has had a strong impact on its application in automobile decoration piece.Simultaneously, motor corporation has proposed corresponding requirement to the performance of associated materials such as mar-proof performance.Therefore, the mar-proof performance that how to improve polypropylene material just becomes this type of exploitation material urgent problem.
The mar-proof performance of relevant raising Vestolen PP 7052 has some reports, has proposed some solutions, fills like Vestolen PP 7052 to strengthen, and improves polyacrylic percent crystallinity, adds the method that some contain organo-siloxane.Foreign patent WO02051933 relates to the mar-proof performance of improving material with the method for mica instead of part talcum powder raising material hardness.Japanese patent laid-open 6-220270 is reported in the polypropylene modification and improves surface hardness through adding nucleator, reaches the purpose of improving mar-proof performance, finds to increase rubber consumption simultaneously and also can improve mar-proof performance.Adopt high-crystallinity polypropylene and talcum powder blend among the Chinese patent CN 1631959A, prepared and have the heat-stable mar-proof talc powder filled polypropylene of high rigidity height.U.S. Pat 5585420 and US5731376 relate to the mar-proof performance that the method that adds high molecular weight siloxane improves material, and be not mentioned rubber toughened.Chinese patent CN1580115A mentions the rubber toughened technology that adopts, and adds the HMW silicone elastomer and nucleator NA-21 makes the rigidity of material and toughness reach good balance.
Summary of the invention
The purpose of this invention is to provide a kind of novel scratch-proof polypropylene matrix material and preparation method thereof.
In order to improve the mar-proof performance of PP composite material, technical scheme of the present invention is in the basic components of polypropylene material, to add to fluoridize organosilicon as anti-stroke of wiping auxiliary agent, thereby improves the mar-proof performance in the PP composite material effectively.This organosilicon of fluoridizing has good dispersiveness, in product, can move to the surface of product, improves the anti scuffing effect and the wear resistance of product.
A kind of novel scratch-proof polypropylene matrix material is mixed with by following raw materials by weight percent:
In the PP composite material system that the present invention was suitable for,
Described Vestolen PP 7052 is a melt flow rate(MFR) (test condition: 230 ℃ * 2.16kg) HOPP between 5～60g/10min or block copolymerization propylene; Wherein the comonomer of block copolymerization propylene is common is ethene; Its content is in the scope of 4～10mol%; The percent crystallinity of HOPP is more than 70%, and degree of isotacticity is greater than 99%.
Described mineral filler is a talcum powder, and its particle size range is 1～10 micron.
Described toughner POE is linear ethylene-octene copolymer, and density is 0.88～0.90g/cm
3, melting index is 0.5～15g/10min (test condition: 190 ℃ * 2.16kg).
Described oxidation inhibitor comprises primary antioxidant and auxiliary anti-oxidant, and primary antioxidant can be selected hindered phenol or thioesters kind antioxidant for use, preferably from 3114,1010 and DSTP in one or more compsn; Auxiliary anti-oxidant can be selected the phosphorite kind antioxidant for use, preferably the combination of one or both in 618 and 168.
Described photostabilizer can be selected hindered amine light stabilizer for use, preferably the compsn of one or more in 944 and 770.
The described organosilicon of fluoridizing has the interface wet performance, and its viscosity in the time of 25 ℃ is 60～300Pas, thisly fluoridizes organosilyl structural formula and is: [RfO (CH
2)
2] CHSiO, wherein the Rf base is the fluoride fat base or the fluoro aryl of line style.
Described other additives are color toner or Masterbatch.
A kind of method for preparing above-mentioned novel scratch-proof polypropylene matrix material the steps include:
1) takes by weighing raw material by weight ratio;
2) with Vestolen PP 7052, talcum powder, toughner POE, fluoridize organosilicon, oxidation inhibitor, photostabilizer or other additives and in super mixer, do to mix 3～5 minutes;
3) raw materials mixed is placed dual-screw-stem machine, through melt extruding, granulation, its technology 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.
The present invention adds a kind of auxiliary agent that can improve mar-proof performance in the basic components of PP composite material, can better PP composite material thereby prepare scratch-resistant.
Advantage of the present invention is:
1, the present invention uses an amount of mar-proof auxiliary agent in composite system, makes polypropylene compound material prepared have better mar-proof performance.
2, polypropylene compound material prepared of the present invention is when guaranteeing the mar-proof performance of material, and each item physical and mechanical property of material is unaffected basically.
3, the method preparation technology who improves the mar-proof performance of PP composite material of the present invention's proposition is simple, production cost is low.
Embodiment
Below in conjunction with embodiment, the present invention is done further explain:
In embodiment and Comparative Examples composite-material formula, used Vestolen PP 7052 is the COPP that Oil of Shanghai Petrochemical Company is produced, and trade names are M2600R.Mineral filler is 5000 order talcum powder, and median size is 2.5 microns.Used toughner POE is linear ethylene-octene copolymer that U.S. Dupont company produces, and trade names Engage 8180, and density is 0.863g/cm3, and melt flow rate(MFR) is 0.5g/10min.The used organosilicon of fluoridizing is the AC-805 fluoride silicon surfactant that Noah's ark (Fugang) chemical material company produces, and it is colourless or faint yellow fluid, and viscosity has 200～300Pas (25 ℃), and the weight percent of its addition is 0.5～4%.Used primary antioxidant is the DSTP that Britain ICE company produces, and trade names are Negonox DSTP, and chemical name is the thio-2 acid octadecyl ester; And BASF AG 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 BASF AG's product, and trade names are Irgafos168, and chemical name is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.Used photostabilizer is 944 of BASF AG's product, and chemical name is for gathering { [6-[(1,1,3, the 3-tetramethyl butyl) amino]]-1,3; 5-triazine-2,4-two [(2,2,6,6;-tetramethyl-4-piperidyl) imino-]-1,6-oneself two the support [(2,2,6,6-tetramethyl--4-piperidyl) imino-]; And BASF AG produce 770, chemical name be pair (2,2,6, the 6-tetramethyl-piperidyl) sebates.
Resin and various additive do to mix in super mixer 3～5 minutes, again in twin screw extruder through melt extruding, granulation, its technology 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 for preparing as stated above, drying is 2～3 hours in 90～100 ℃ convection oven, and then the particulate material that drying is good carries out the injection molding sample preparation on injection moulding machine.
Mar-proof performance test: injection molding size of sample 150 * 100 * 3.2mm; Use scratch hardness tester ERICHSEN430P-I load to be that 10N, nib diameter are that 1mm carries out scratch test on the model surface, cut is 2mm at interval; 20 lines of each stroke of vertical and horizontal; The color and luster that grid material is drawn in the color measurement system testing of adopting Japanese Minolta company to produce changes, the Δ L value of recording materials, thereby the mar-proof performance of discriminating material.
Melt flow rate(MFR) (MFR) is measured: undertaken by the ISO1183 standard, probe temperature is 230 ℃, load 2.16kg;
The tensile property test: undertaken by ISO 527-2 standard, specimen size is 170*10*4mm, and draw speed is 50mm/min;
The bending property test: undertaken by ISO 178 standards, specimen size is 80*10*4mm, and rate of bending is 2mm/min, and span is 64mm, and modulus in flexure is undertaken by tangential direction;
The simple beam impact strength test: undertaken by ISO 179 standards, specimen size is 80*6*4mm, and notch depth is 1/3rd of a sample thickness;
Comprehensive mechanical performance is passed judgment on through the numerical value of shock strength, notched Izod impact strength, tensile strength, flexural strength and the modulus in flexure of test gained.
The mar-proof performance of material is according to the PV3952 standard code, passes judgment on the photostabilization grade according to the value of the colour-change scale Δ L of material surface.The numerical value of Δ L is more little, and the mar-proof performance of expression material is good more, and mar-proof grade is also just high more.Example formulations and each item The performance test results see the following form:
Table 1 embodiment 1-6 and Comparative Examples 1-3 material prescription table (weight %)
Table 2 embodiment 1-6 and Comparative Examples 1-3 material property table
Contrast from embodiment 1-4 and Comparative Examples 1; Embodiment 5 and Comparative Examples 2 and embodiment 6 can find out with the contrast of Comparative Examples 3; The mar-proof performance of fluoridizing the PP composite material system that organosilicon fills toughner and talcum powder improves a lot, wherein add 2% o'clock comparatively remarkable to the mar-proof performance that improves the PP material.At this moment, material not only possesses good mar-proof performance, and the basic physical and mechanical property of material also can keep preferably simultaneously.
Claims (10)
1. novel scratch-proof polypropylene matrix material is characterized in that: be mixed with by following raw materials by weight percent:
2. novel scratch-proof polypropylene matrix material according to claim 1 is characterized in that: described Vestolen PP 7052 is HOPP or the block copolymerization propylene of melt flow rate(MFR) between 5～60g/10min under the 2.16kg test condition at 230 ℃.
3. novel scratch-proof polypropylene matrix material according to claim 2 is characterized in that: the comonomer of described block copolymerization propylene is an ethene, and its content is in the scope of 4～10mol%; The percent crystallinity of HOPP is more than 70%, and degree of isotacticity is greater than 99%.
4. novel scratch-proof polypropylene matrix material according to claim 1 is characterized in that: described mineral filler is a talcum powder, and its particle size range is 1～10 micron.
5. novel scratch-proof polypropylene matrix material according to claim 1 is characterized in that: described toughner POE is linear ethylene-octene copolymer, and density is 0.88～0.90g/cm
3At 190 ℃, under the test condition of 2.16kg, its melting index is 0.5～15g/10min.
6. novel scratch-proof polypropylene matrix material according to claim 1; It is characterized in that: described oxidation inhibitor comprises primary antioxidant and auxiliary anti-oxidant; Primary antioxidant is selected hindered phenol or thioesters kind antioxidant for use, and auxiliary anti-oxidant is selected the phosphorite kind antioxidant for use.
7. novel scratch-proof polypropylene matrix material according to claim 6 is characterized in that: described primary antioxidant be selected from 3114,1010 and DSTP in one or more compsn; Auxiliary anti-oxidant is selected from one or both the combination in 618 and 168.
8. novel scratch-proof polypropylene matrix material according to claim 1, it is characterized in that: described photostabilizer is a hindered amine light stabilizer, is selected from one or more the compsn in 944 and 770.
9. novel scratch-proof polypropylene matrix material according to claim 1 is characterized in that: the described organosilicon of fluoridizing, have the interface wet performance, and its viscosity in the time of 25 ℃ is 60～300Pas, thisly fluoridizes organosilyl structural formula and is: [RfO (CH
2)
2] CHSiO, wherein the Rf base is the fluoride fat base or the fluoro aryl of line style.
10. a method for preparing the said novel scratch-proof polypropylene matrix material of claim 1 is characterized in that: the steps include:
1) takes by weighing raw material by weight ratio;
2) with Vestolen PP 7052, talcum powder, toughner POE, fluoridize organosilicon, oxidation inhibitor, photostabilizer or other additives and in super mixer, do to mix 3～5 minutes;
3) raw materials mixed is placed dual-screw-stem machine, through melt extruding, granulation, its technology 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.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766299A (en) * | 2012-08-01 | 2012-11-07 | 长沙达联塑料有限公司 | Anti-impacting anti-ageing modified polypropylene material and preparation method thereof |
| CN104119607A (en) * | 2014-06-26 | 2014-10-29 | 合肥和安机械制造有限公司 | Special filler for high-wear-resistant cable sheath material and preparation method thereof |
| CN105462076A (en) * | 2015-12-17 | 2016-04-06 | 东莞市顶好新材料科技有限公司 | Wear-resisting stable PP electroplated substrate based on nanometer clay and preparing method thereof |
| CN109880106A (en) * | 2019-03-04 | 2019-06-14 | 浙江新安化工集团股份有限公司 | A kind of super high molecular weight modified polyorganosiloxane, preparation method and the application in plastic processing |
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| EP0682679B1 (en) * | 1993-02-03 | 1997-12-10 | BASF Aktiengesellschaft | Scratch resistant polymer compositions |
| CN101293893A (en) * | 2007-04-29 | 2008-10-29 | 上海远东氟材料技术有限公司 | Fluorosiloxane midbody for hard surface dressing, prepraring method and method for preparing fluorosiloxane thereof |
| CN101698726A (en) * | 2009-11-04 | 2010-04-28 | 苏州旭光聚合物有限公司 | Scratch-resistant modified polypropylene composite material and preparation method thereof |
| CN101759913A (en) * | 2008-11-21 | 2010-06-30 | 上海普利特复合材料股份有限公司 | Novel scratch-proof polypropylene material and preparation method thereof |
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2011
- 2011-12-26 CN CN2011104421260A patent/CN102558677A/en active Pending
Patent Citations (4)
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| EP0682679B1 (en) * | 1993-02-03 | 1997-12-10 | BASF Aktiengesellschaft | Scratch resistant polymer compositions |
| CN101293893A (en) * | 2007-04-29 | 2008-10-29 | 上海远东氟材料技术有限公司 | Fluorosiloxane midbody for hard surface dressing, prepraring method and method for preparing fluorosiloxane thereof |
| CN101759913A (en) * | 2008-11-21 | 2010-06-30 | 上海普利特复合材料股份有限公司 | Novel scratch-proof polypropylene material and preparation method thereof |
| CN101698726A (en) * | 2009-11-04 | 2010-04-28 | 苏州旭光聚合物有限公司 | Scratch-resistant modified polypropylene composite material and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766299A (en) * | 2012-08-01 | 2012-11-07 | 长沙达联塑料有限公司 | Anti-impacting anti-ageing modified polypropylene material and preparation method thereof |
| CN102766299B (en) * | 2012-08-01 | 2014-04-16 | 长沙达联塑料有限公司 | Anti-impacting anti-ageing modified polypropylene material and preparation method thereof |
| CN104119607A (en) * | 2014-06-26 | 2014-10-29 | 合肥和安机械制造有限公司 | Special filler for high-wear-resistant cable sheath material and preparation method thereof |
| CN105462076A (en) * | 2015-12-17 | 2016-04-06 | 东莞市顶好新材料科技有限公司 | Wear-resisting stable PP electroplated substrate based on nanometer clay and preparing method thereof |
| CN105462076B (en) * | 2015-12-17 | 2018-08-07 | 东莞市顶好新材料科技有限公司 | Wear-resisting stable PP electroplating substrates based on nanoclay and preparation method thereof |
| CN109880106A (en) * | 2019-03-04 | 2019-06-14 | 浙江新安化工集团股份有限公司 | A kind of super high molecular weight modified polyorganosiloxane, preparation method and the application in plastic processing |
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Application publication date: 20120711 |