CN116444899B - Polypropylene compound and preparation method and application thereof - Google Patents
Polypropylene compound and preparation method and application thereof Download PDFInfo
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- CN116444899B CN116444899B CN202310429225.8A CN202310429225A CN116444899B CN 116444899 B CN116444899 B CN 116444899B CN 202310429225 A CN202310429225 A CN 202310429225A CN 116444899 B CN116444899 B CN 116444899B
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- 229920001155 polypropylene Polymers 0.000 title claims abstract description 116
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 114
- -1 Polypropylene Polymers 0.000 title claims abstract description 109
- 150000001875 compounds Chemical class 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229920001577 copolymer Polymers 0.000 claims abstract description 77
- 229920005604 random copolymer Polymers 0.000 claims abstract description 36
- 239000003381 stabilizer Substances 0.000 claims abstract description 29
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000005977 Ethylene Substances 0.000 claims abstract description 25
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims abstract description 11
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003963 antioxidant agent Substances 0.000 claims description 43
- 230000003078 antioxidant effect Effects 0.000 claims description 33
- 239000000155 melt Substances 0.000 claims description 29
- 238000012360 testing method Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 19
- 239000002131 composite material Substances 0.000 claims description 15
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 13
- AVXURJPOCDRRFD-UHFFFAOYSA-N hydroxylamine group Chemical group NO AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 9
- 238000002347 injection Methods 0.000 claims description 9
- 239000007924 injection Substances 0.000 claims description 9
- 239000012964 benzotriazole Substances 0.000 claims description 8
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 3
- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 claims description 2
- 238000005453 pelletization Methods 0.000 claims description 2
- 239000006096 absorbing agent Substances 0.000 claims 1
- VVOLVFOSOPJKED-UHFFFAOYSA-N copper phthalocyanine Chemical compound [Cu].N=1C2=NC(C3=CC=CC=C33)=NC3=NC(C3=CC=CC=C33)=NC3=NC(C3=CC=CC=C33)=NC3=NC=1C1=CC=CC=C12 VVOLVFOSOPJKED-UHFFFAOYSA-N 0.000 claims 1
- 238000002834 transmittance Methods 0.000 abstract description 21
- 238000001746 injection moulding Methods 0.000 abstract description 18
- 239000000203 mixture Substances 0.000 abstract description 10
- 238000005191 phase separation Methods 0.000 abstract description 6
- 238000010008 shearing Methods 0.000 abstract description 4
- 239000002861 polymer material Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 description 19
- 239000011347 resin Substances 0.000 description 19
- 238000002844 melting Methods 0.000 description 16
- 230000008018 melting Effects 0.000 description 16
- 239000000463 material Substances 0.000 description 15
- 239000002994 raw material Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 8
- 101000872084 Danio rerio Delta-like protein B Proteins 0.000 description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 6
- 230000004075 alteration Effects 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 6
- 239000000806 elastomer Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- RBTKNAXYKSUFRK-UHFFFAOYSA-N heliogen blue Chemical compound [Cu].[N-]1C2=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=NC([N-]1)=C(C=CC=C3)C3=C1N=C([N-]1)C3=CC=CC=C3C1=N2 RBTKNAXYKSUFRK-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000007921 spray Substances 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- DYPWCFYFKMNBTB-UHFFFAOYSA-N C1C(C)S1.C=C Chemical compound C1C(C)S1.C=C DYPWCFYFKMNBTB-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000004611 light stabiliser Substances 0.000 description 2
- 238000002464 physical blending Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
- SSADPHQCUURWSW-UHFFFAOYSA-N 3,9-bis(2,6-ditert-butyl-4-methylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C)=CC(C(C)(C)C)=C1OP1OCC2(COP(OC=3C(=CC(C)=CC=3C(C)(C)C)C(C)(C)C)OC2)CO1 SSADPHQCUURWSW-UHFFFAOYSA-N 0.000 description 1
- PZRWFKGUFWPFID-UHFFFAOYSA-N 3,9-dioctadecoxy-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound C1OP(OCCCCCCCCCCCCCCCCCC)OCC21COP(OCCCCCCCCCCCCCCCCCC)OC2 PZRWFKGUFWPFID-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000006855 networking Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920005633 polypropylene homopolymer resin Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229940124543 ultraviolet light absorber Drugs 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polypropylene compound, a preparation method and application thereof, and belongs to the technical field of high polymer materials. The polypropylene compound comprises the following components in parts by weight: 60-96 parts of random copolymer polypropylene; 2-20 parts of ethylene propylene copolymer; 2-20 parts of propylene butene copolymer; 0.1-0.9 part of stabilizer; 0-0.05 part of color difference regulator; in the random copolymer polypropylene, the mol content of ethylene is 1% -3.9%; in the ethylene-propylene copolymer, the molar content of ethylene is 4% -16%; in the propylene-butene copolymer, the molar content of butene is 5% -18%. The polypropylene compound of the invention adjusts the light transmittance through the mixture of the ethylene propylene copolymer, the propylene butylene copolymer and the random copolymer polypropylene, almost has no microscopic phase separation under strong shearing, and almost has no vacuum hole after injection molding of small gate or self-release gate parts.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polypropylene compound and a preparation method and application thereof.
Background
With the development of electric, intelligent and networking in the automotive industry, consumers have increasingly higher requirements on automotive interior materials, and in order to meet individual demands of consumers, decorative lamps, atmosphere lamps and the like have been widely applied to interior door panels, instrument panels, upright posts and other interior parts, and development and application of light-transmitting parts are followed. The polypropylene (PP) has the advantages of low density, excellent mechanical property, low cost, easy processing, easy recycling and the like, is widely applied to automobile interior and exterior decorative parts, belongs to semitransparent polymer materials, can be modified to adjust the transparency, and can be applied to the light-transmitting parts.
The prior art discloses a uniform light-transmitting polypropylene composition, which improves the light-transmitting uniformity of polypropylene through ethylene propylene sulfide with gel content more than or equal to 85wt%, and has smaller light transmittance and haze difference of less than or equal to 4.3 and haze difference of less than or equal to 0.44 under different injection molding conditions. The polypropylene composition disclosed by the above technology has uniform light transmission performance, but the material is added with ethylene propylene sulfide elastomer by means of post physical blending modification, and the elastomer is dispersed in a polypropylene matrix like islands in a sea-island structure to form a heterogeneous morphology. In order to save raw materials, cost, labor cost and the like, the current automobile parts are designed with small gates or self-release gates, and polypropylene compound melts of the physically mixed elastomer are easy to form a spraying state when passing through the gates, microscopic phase separation is generated, and the defects that vacuum holes and the like are easy to form after the polypropylene melts enter a suddenly-enlarged cavity are particularly obvious for products with larger wall thickness change.
In view of the above, it is desirable to provide a polypropylene composite that reduces the creation of vacuum holes in the interior of a part after injection molding of a small gate or self-releasing gate part.
Disclosure of Invention
The invention aims to overcome the defect and the defect that vacuum holes can be generated in a finished piece when the traditional uniform light-transmitting polypropylene composition is used for injection molding of a small gate or a self-release gate finished piece, and provides a polypropylene compound which takes random copolymer polypropylene as a matrix, and ethylene propylene copolymer and propylene butene copolymer are added for mixing and adjusting light-transmitting performance.
It is a further object of the present invention to provide a process for the preparation of polypropylene compounds.
It is a further object of the present invention to provide the use of a polypropylene composite for the preparation of light transmissive polypropylene injection molded articles.
The above object of the present invention is achieved by the following technical scheme:
the polypropylene compound comprises the following components in parts by weight:
in the random copolymer polypropylene, the mol content of ethylene is 1% -3.9%;
in the ethylene-propylene copolymer, the molar content of ethylene is 4% -16%;
in the propylene-butene copolymer, the molar content of butene is 5% -18%.
The polypropylene compound adopts the random copolymer polypropylene as a matrix, the random copolymer polypropylene has no obvious crystallization area and amorphous area, has the characteristics of homogeneity and no microscopic phase separation, and adjusts the light transmittance through the mixing of the ethylene-propylene copolymer, the propylene-butylene copolymer and the random copolymer polypropylene.
In practical application, the light transmittance can be regulated and controlled by the random copolymerization of polypropylene, the ethylene-propylene copolymer and the propylene-butylene copolymer, and particularly, an elastomer or a filler can be not added or added in a very small amount, and the elastomer or the filler is not required to be added in a physical blending mode, so that the generation of microscopic phase separation can be prevented, and a large number of vacuum holes can be further prevented.
The test standard for the molar content of ethylene in the random copolymer polypropylene and ethylene propylene copolymer was Q/SY DS 0240.118-2004.
The method for testing the molar content of the butene in the propylene butene copolymer is an infrared spectrometry method, and the characteristic absorption peak of the butene is 766cm -1 Selecting 806cm -1 The absorption peak of polypropylene is a reference peak, and the absorbance ratio (x=a 766 /A 806 ) The butene content was calculated according to the formula: butene content = -5.410X 2 +28.485X+0.0113：
Preferably, the melt mass flow rate of the random copolymer polypropylene is 0.2-44g/10min under the conditions of 230 ℃ and 2.16kg, and the test standard is GB/T3682-2018.
More preferably, the melt mass flow rate of the random copolymer polypropylene is 6-30g/10min at 230 ℃ and 2.16kg, and the test standard is GB/T3682-2018.
Preferably, the melt mass flow rate of the ethylene propylene copolymer is 1.2-100g/10min under the conditions of 230 ℃ and 2.16kg, and the test standard is GB/T3682-2018.
More preferably, the ethylene propylene copolymer has a melt mass flow rate of 2-50g/10min at 230℃and 2.16kg, with a test standard of GB/T3682-2018.
Preferably, the ethylene propylene copolymer has a molar content of ethylene of 9% to 15%.
The test criteria for the molar content of propylene/ethylene in the ethylene propylene copolymer were: SH/T1800-2016.
Preferably, the propylene butene copolymer has a melt mass flow rate of 2.8-19.8g/10min at 230 ℃ and 2.16kg, and the test standard is GB/T3682-2018.
More preferably, the propylene butene copolymer has a melt mass flow rate of 5-15g/10min at 230 ℃ and 2.16kg, with a test standard of GB/T3682-2018.
Preferably, the color difference regulator is beta crystal form copper phthalocyanine blue.
When a polypropylene compound is used for injection molding a small gate or a self-release gate workpiece, because strong shearing is generated at the small gate, the molded workpiece visually presents a 'staleness' compared with a raw material, and therefore, in order to reduce the 'staleness', improve the 'freshness', the change of chromatic aberration delta B needs to be controlled, namely, compared with the raw material, the less the chromatic aberration delta B is increased, the less the staleness is, and the more the freshness is strong.
According to the invention, the beta-crystal copper phthalocyanine blue with stable crystal green phase is added, so that the color difference delta B between the injection molded part and the raw material can be reduced, and the freshness of the raw material can be maintained for the injection molded part.
Preferably, the stabilizer comprises an antioxidant and/or an ultraviolet absorber, wherein the antioxidant is a hydroxylamine antioxidant and/or a phosphite antioxidant, and the ultraviolet absorber is a benzotriazole ultraviolet absorber.
The antioxidant can play an antioxidant role in the injection molding process. Because the hydroxylamine antioxidant and the phosphite antioxidant do not comprise alkylphenol structures, the freshness of the molded parts can be improved.
Preferably, in the stabilizer, the mass ratio of hydroxylamine antioxidant, phosphite antioxidant and benzotriazole ultraviolet absorber is (1-2): (1-2): 1.
preferably, the purity of the stabilizer is greater than or equal to 99.5%.
The high-purity stabilizer obtained after purification has little free phenol micromolecular substances, and little color-changing substances can be generated under the shearing heat caused by a small sprue, thereby being beneficial to reducing the color difference delta B between a workpiece and raw materials after injection molding and improving the freshness of the workpiece.
The purification method of the stabilizer may be a melt-crystallization method.
Preferably, the hydroxylamine antioxidant has a melting point of 90 ℃ or more and a molecular weight of 500 or more.
The melting point and the molecular weight of the hydroxylamine antioxidant influence the thermal stability of the material, and the hydroxylamine antioxidant is used as a main antioxidant and compounded with phosphite antioxidants, so that the long-acting thermal stability of the material is improved, and the precipitation phenomenon of the hydroxylamine antioxidant in the material processing and using processes is reduced through the selection of the melting point and the molecular weight, and the freshness of a finished product is maintained.
Preferably, the melting point of the phosphite antioxidant is 50-60 ℃, and the molecular weight is more than or equal to 700;
the melting point and molecular weight of phosphite antioxidants affect the thermal stability of the material, and the phosphite antioxidants are used as auxiliary antioxidants to be compounded with hydroxylamine antioxidants, so that the thermal stability of the material in the processing process is improved, and the phosphite antioxidants are reduced to act and avoid the generation of discolored trace substances by selecting the types, the melting point and the molecular weight, so that the freshness of the product is maintained.
Preferably, the melting point of the benzotriazole ultraviolet absorber is 100-110 ℃, and the 500nm light transmittance is more than 98%.
The melting point and the light transmittance of the benzotriazole ultraviolet absorber influence the light stability and the light transmittance of the compound, and reduce the influence on the light transmittance of polypropylene.
The invention also provides a preparation method of the polypropylene compound, which comprises the following steps:
adding the stabilizer, the chromatic aberration regulator, the random copolymer polypropylene, the ethylene-propylene copolymer and the propylene-butylene copolymer into a high-speed mixer for uniform mixing, adding into a main feeding port of a double-screw extruder, carrying out melt blending at 180-230 ℃, extruding and granulating to obtain the polypropylene compound.
Preferably, the preparation method of the polypropylene compound comprises the following steps: grinding stabilizer and color difference regulator, mixing with atactic copolymerized polypropylene, ethylene-propylene copolymer and propylene-butylene copolymer, adding into double screw extruder, melt blending at 180-230 deg.c, extruding and pelletizing to obtain polypropylene composite.
Preferably, the milling time is not less than 1 minute.
The invention adopts the method of pre-grinding the stabilizer and the color difference regulator for more than or equal to 1 minute and then mixing with other components, solves the problem of agglomeration in the processing process of the stabilizer and the color difference regulator, is more beneficial to improving the dispersion uniformity of the micro phthalocyanine blue in the material after the addition, ensures that the color b value of the material is uniform and stable, and further improves the freshness of the material.
The polypropylene compound prepared by the invention hardly generates vacuum holes after injection molding of small gates or self-release gate workpieces, can be widely applied to preparation of plastic products, and particularly protects application of the polypropylene compound in preparation of light-transmitting polypropylene injection molded products, such as lighting lamps and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses a polypropylene compound, which adopts random copolymer polypropylene as a matrix, and adjusts light transmittance through mixing ethylene propylene copolymer, propylene butene copolymer and random copolymer polypropylene, little micro phase separation is generated under strong shearing, and little vacuum hole is generated after injection molding of small gate or self-release gate workpieces.
The polypropylene compound is used as a raw material, and on the premise that the light transmittance and the haze are both 50-90% and the weather resistance delta E is less than or equal to 1.0, the injection molding product of the injection molding small gate or the self-release gate only has small and less vacuum holes or no vacuum holes, and the vacuum hole score can reach 90-100 minutes; and the color difference delta B between the injection molded part and the raw material is less than 0.83.
Drawings
Fig. 1 shows the appearance without vacuum holes.
Fig. 2 shows an appearance with small and few vacuum holes.
Fig. 3 shows the appearance of a large number of vacuum holes.
Fig. 4 shows an appearance with a large and small vacuum hole.
Fig. 5 shows the appearance of a large number of vacuum holes.
Detailed Description
The invention will be further described with reference to the following specific embodiments, but the examples are not intended to limit the invention in any way. Raw materials reagents used in the examples of the present invention are conventionally purchased raw materials reagents unless otherwise specified.
Random copolymer polypropylene resin 1: the mass flow rate of melt at 230 ℃ and 2.16kg of PP-R RP348R is 25g/10min, the mol content of ethylene is 1.6 percent, and the melt is the medium sea shell;
random copolymer polypropylene resin 2: the random copolymer polypropylene resin PP-R R200P-3702 has a melt mass flow rate of 0.2g/10min at 230 ℃ and 2.16kg, a molar content of ethylene of 3.5%, and Korea dawn;
random copolymer polypropylene resin 3: the mass flow rate of melt of the random copolymer polypropylene resin PP RP342N at 230 ℃ and 2.16kg is 9.6g/10min, the mol content of ethylene is 2.9 percent, and Lanzhou petrochemical industry;
polypropylene resin 4: the segmented polypropylene resin K7726 has a melt mass flow rate of 26g/10min at 230 ℃ and 2.16kg, and ethylene molar content of 20.6 percent, which is obtained by China petrochemical company, yanshan petrochemical company;
polypropylene resin 5: the melt mass flow rate of the homo-polypropylene resin Z30S under the conditions of 230 ℃ and 2.16kg is 25g/10min, the ethylene molar content is 0 percent, and the North Hua Jin chemical industry group Co., ltd;
random copolymer polypropylene resin 6: the mass flow rate of melt of the random copolymer polypropylene resin PP J-590S at 230 ℃ and 2.16kg is 44g/10min, the molar content of ethylene is 1.3 percent, and the like is happy day chemistry;
random copolymer polypropylene resin 7: the random copolymer polypropylene resin PP R140M has a melt mass flow rate of 6g/10min at 230 ℃ and 2.16kg, and ethylene mole content of 2.1%, korea SK;
ethylene propylene copolymer 1: vistamaxx 6202FL, melt mass flow rate at 230 ℃,2.16kg, 20g/10min, ethylene molar content 15%, exxon Mobil;
ethylene propylene copolymer 2: vistamaxx 3020FL, a melt mass flow rate of 1.2g/10min at 230 ℃,2.16kg, an ethylene molar content of 11%, exxon mobil;
ethylene propylene copolymer 3: vistamaxx 3980FL, a melt mass flow rate of 8g/10min at 230 ℃,2.16kg, a molar content of ethylene of 9%, exxon mobil;
ethylene propylene copolymer 4: vistamaxx 6502, melt mass flow rate at 230 ℃,2.16kg, 45g/10min, ethylene molar content 13%, exxon mobil;
ethylene propylene copolymer 5: vistamaxx 3588FL, melt mass flow rate at 230 ℃,2.16kg, 8g/10min, ethylene molar content 4%, exkesen mobil;
ethylene propylene copolymer 6: vistamaxx 6902, melt mass flow rate at 230 ℃,2.16kg at 100g/10min, ethylene molar content 12%, exxon mobil;
ethylene alpha olefin (octene) copolymer: POE 8150, wherein the mass flow rate of the melt under the condition of 2.16kg at 230 ℃ is 1.2g/10min, and the ceramic is a ceramic;
propylene butene copolymer 1: PP M1500B, melt mass flow rate at 230 ℃ and 2.16kg is 13g/10min, molar content of butene is 17%, and Shanghai petrochemical;
propylene butene copolymer 2: cefor SRD104, melt mass flow rate under the condition of 230 ℃ and 2.16kg is 5.0g/10min, the molar content of butene is 11 percent, and shell is set;
propylene butene copolymer 3: PP F280B, the mass flow rate of the melt under the conditions of 230 ℃ and 2.16kg is 2.8g/10min, the molar content of butene is 15 percent, and Shanghai petrochemical industry is realized;
propylene butene copolymer 4: PPR-MT18-S, the mass flow rate of the melt under the condition of 2.16kg at 230 ℃ is 19.8g/10min, the molar content of butene is 5%, and the melt is made into a thick petrochemical product;
stabilizer 1 is prepared from hydroxylamine antioxidant, phosphite antioxidant, benzotriazole ultraviolet absorbent according to a proportion of 1:1:1, wherein
Hydroxylamine antioxidants: antioxidant Revonox 420, melting point 96-98 ℃, molecular weight 538;
phosphite antioxidants: antioxidant 618, melting point 54-56 ℃, molecular weight 733;
benzotriazole ultraviolet light absorber: ultraviolet absorbent UV-5411, melting point 101-106 ℃,500nm light transmittance >98%;
the stabilizers are commercially available and are purified for a plurality of times by a melting-crystallization method until the purity is more than or equal to 99.5%, and all the examples and the comparative examples are the same;
stabilizer 2: hindered phenol type antioxidant, thioether type antioxidant, aryl phosphite ester antioxidant, ultraviolet absorber and hindered amine light stabilizer are formed in a ratio of 1:1:1:1:1,
wherein the hindered phenol antioxidant is antioxidant 3114, melting point is 218-220 ℃, and molecular weight is 784;
the thio-ether antioxidant is antioxidant 412S, the melting point is 47 ℃, and the molecular weight is 1162;
the phosphite antioxidant is antioxidant PEP-36, melting point 234-240 ℃ and molecular weight 633;
the ultraviolet absorber is UV-531; melting point 48-49 deg.c, 500nm light transmittance not less than 95%;
the hindered amine light stabilizer is UV-3853; melting point 29 ℃,500nm light transmittance is more than or equal to 85%;
the stabilizers are commercially available and all require multiple purifications by melt-crystallization to a purity of 99.5% or more, and all examples and comparative examples are the same.
Color difference regulator 1: beta crystal form copper phthalocyanine blue: heliogen Blue K7104LW, basff;
color difference regulator 2: alpha crystal form copper phthalocyanine blue: heliogen Blue L6930, basoff;
color difference regulator 3: epsilon crystal form copper phthalocyanine blue: heliogen Blue L6700F, basoff;
examples 1 to 19
The polypropylene compound comprises the following components in parts by weight:
random copolymer polypropylene; an ethylene propylene copolymer; propylene butene copolymers; stabilizers and color difference modifiers, wherein the specific contents of the components are shown in table 1 below.
Table 1 Polypropylene composite composition (in parts by weight) of each example
Table 1, below
The preparation method of the polypropylene compound specifically comprises the following steps:
adding the stabilizer and the chromatic aberration regulator into a grinder for mixing and grinding uniformly, then adding the mixture and the random copolymer polypropylene, the ethylene-propylene copolymer and the propylene-butylene copolymer into a high-speed mixer for mixing uniformly, adding the mixture into a main feeding port of a double-screw extruder, carrying out melt blending at 180-230 ℃, extruding and granulating to obtain the polypropylene compound.
Example 20
The polypropylene composite, which has the same amount of each component as in example 1, is prepared by the following method, which is different from example 1:
the preparation method of the polypropylene compound specifically comprises the following steps:
adding the stabilizer, the chromatic aberration regulator, the random copolymer polypropylene, the ethylene-propylene copolymer and the propylene-butylene copolymer into a high-speed mixer for uniform mixing, adding into a main feeding port of a double-screw extruder, carrying out melt blending at 180-230 ℃, extruding and granulating to obtain the polypropylene compound.
Comparative examples 1 to 12
The polypropylene compound comprises the following components in parts by weight:
random copolymer polypropylene; an ethylene propylene copolymer; propylene butene copolymers; stabilizers and color difference modifiers, wherein the specific contents of the components are shown in table 2 below.
Table 2 Polypropylene composite composition (in parts by weight) of each comparative example
| Component (A) | 1 | 2 | 3 | 4 | 5 |
| Random copolymer Polypropylene resin 1 | 80 | 80 | 80 | 80 | 80 |
| Ethylene propylene copolymer 1 | 15 | 35 | / | 15 | 0 |
| POE | / | / | 15 | / | / |
| Propylene butene copolymer 1 | 35 | 5 | 5 | 0 | 5 |
| Stabilizer 1 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 |
| Color difference regulator 1 | 0.001 | 0.001 | 0.001 | 0.001 | 0.001 |
Continuous table 2
| Component (A) | 6 | 7 | 8 | 9 | 10 | 11 | 12 |
| Random copolymer Polypropylene resin 1 | 100 | / | / | 80 | 80 | 80 | 80 |
| Polypropylene resin 4 | / | 80 | / | / | / | / | / |
| Polypropylene resin 5 | / | / | 80 | / | / | / | / |
| Ethylene propylene copolymer 1 | 0 | 15 | 15 | 15 | 15 | 20 | 0 |
| Propylene butene copolymer 1 | 0 | 5 | 5 | 5 | 5 | 0 | 20 |
| Stabilizer 1 | 0.6 | 0.6 | 0.6 | 1.5 | 0.6 | 0.6 | 0.6 |
| Color difference regulator 1 | 0.001 | 0.001 | 0.001 | 0.001 | 0.1 | 0.001 | 0.001 |
The preparation method of the polypropylene compound specifically comprises the following steps:
adding the stabilizer and the chromatic aberration regulator into a grinder for mixing and grinding uniformly, then adding the mixture and random copolymer polypropylene (or polypropylene), ethylene-propylene copolymer (or POE) and propylene-butylene copolymer (or none) into a high-speed mixer for mixing uniformly, adding the mixture into a main feeding port of a double-screw extruder, carrying out melt blending at 180-230 ℃, extruding and granulating to obtain the polypropylene compound.
Result detection
And (3) the polypropylene compound is molded into a color plate and a strip-shaped sample plate by an injection molding method.
The polypropylene compounds of the above examples and comparative examples were tested by the following performance test methods:
vacuum holes: visual evaluation, scoring according to the number and the size of the vacuum holes, wherein 100 is divided into no vacuum holes (shown in figure 1); 90 are divided into small and small (as shown in fig. 2); 80 is divided into small and large (as shown in fig. 3), 70 is divided into large and small (as shown in fig. 4), and 60 is divided into large and large (as shown in fig. 5). Wherein 90 or more is an acceptable state, allowing intermediate values such as 95, 85, 75, 65, etc.
L, a and b values were measured in accordance with the 4.64CIE LAB color space of GB/T5698-2001.
Δb: to simulate the shear heat generated at the small gate, the plaques were injection molded at 180 ℃ and 230 ℃ respectively, and their color difference values were tested to characterize freshness as Δb, where Δb=b value (230 ℃) to B value (180 ℃). The smaller Δb, the better the freshness sensation. The b value was measured in accordance with the 4.64CIE LAB color space of GB/T5698-2001.
Transmittance/haze: test method referring to B method in GB/T2410-2008, the thickness of the sample plate is 2mm, the accurate value of light transmittance and haze is 1%, and the light transmittance and haze are between 50% and 90% as the best result.
Weather resistance Δe: testing L value and a value of sample plateAnd b, marking as a color difference value before test, wherein weather-proof test conditions are as follows: the black board temperature (38+/-3) DEG C, the box air temperature (38+/-3) DEG C and the relative humidity (95+/-5)% are tested, and the black board is operated for 1 hour; the blackboard temperature (89+/-3) DEG C, the box air temperature (62+/-2) DEG C and the relative humidity (50+/-5)% under the test condition, and the operation is carried out for 3.8 hours of illumination circulation; radiation intensity (1.2.+ -. 0.02) W/m 2 Wavelength 420nm, test time 624h. And after aging, testing the L value, the a value and the b value of the template again, marking the L value, the a value and the b value as the color difference value after testing, and comparing the delta E value before and after testing the template. Δe= [ (Δl) 2 +(△A) 2 +(△B) 2 ] 1/2 Wherein Δl=l value (post test) -L value (pre test), Δa=a value (post test) -a value (pre test), Δb=b value (post test) -B value (pre test).
Δl, Δa, and Δb represent changes in color at L value (luminance), a value (red-green), and B value (yellow-blue), respectively. The patent adopts the LAB mode to represent the color difference, and is the LAB mode established in 1976 by the International Commission on illumination, namely CIE LAB color space. Wherein Δe characterizes the overall color change, Δb values represent the yellowish green change, and the smaller the number, the smaller the change, and the better the freshness.
Specific test results are shown in Table 3 below:
as can be seen from the data, the polypropylene compound prepared in the embodiments 1-20 is adopted, and under the premise that the light transmittance and the haze are both 50-90% and the weather resistance delta E is less than or equal to 1.0, the strip-shaped sample plate of the injection small gate or the self-release gate only has small and less vacuum holes or no vacuum holes, and the vacuum hole score can reach 90-100 minutes; and the color difference delta B between the injection molded part and the raw material is less than 0.83.
As can be seen from example 1 and comparative example 1, an excessive amount of propylene-butene copolymer resulted in excessive haze.
It can be found from examples 1 and 2 that an excessive amount of the ethylene propylene copolymer results in too low light transmittance and haze.
It can be seen from examples 1 and 3 that with conventional elastomer POE, phase separation occurs through small gates during injection molding, resulting in the appearance of large and much larger vacuum holes, due to the "islands-in-the-sea" structure that exists after blending with polypropylene.
It was found from examples 1 and comparative examples 4 to 6 that the reduction of the ethylene propylene copolymer or propylene butene copolymer resulted in deterioration of the compatibility of the polypropylene compound, and that not only vacuum holes were formed, but also the light transmittance and haze were too low.
As can be seen from examples 1 and comparative examples 7 to 8, the use of homo-or co-polypropylene with high crystallinity instead of random co-polypropylene, which has strong orientation phenomenon through small gates, orientation crystallization after cooling and continuous progress of crystallization, and continuous molecular chain movement inside the outer layer of the article after cooling, resulted in large and numerous vacuum holes.
It was found from examples 1 and 9 that the stabilizer was excessive and the weather resistance was greatly improved, but that excessive stabilizer means that more discoloration was generated during injection molding and precipitation occurred, resulting in an excessively large Δb value.
As can be seen from examples 1 and 10, the excessive amount of the color difference adjusting agent, which is an organic substance, is inferior in heat resistance and weather resistance, resulting in excessive increase in both the DeltaB value and weather resistance DeltaE.
As can be seen from examples 1 and 11, the propylene-butene copolymer was not contained, and when the ethylene-propylene copolymer was 20 parts, the polypropylene was inferior in compatibility with the ethylene-propylene copolymer, and not only vacuum holes were formed, but also light transmittance and haze were too low.
As can be seen from examples 1 and 12, when the ethylene-propylene copolymer was not contained and the propylene-butene copolymer was 20 parts, the polypropylene was inferior in compatibility with the propylene-butene copolymer, and not only vacuum holes were formed, but also haze was too low.
As can be seen from examples 1, 2, 3, 4, 12 and 13, the ethylene propylene copolymer has a melt mass flow rate in the range of 2 to 50g/10min, fewer vacuum holes, smaller DeltaB number and better freshness of the material. Within the above range, the higher the melt mass flow rate of the ethylene-propylene copolymer, the lower the shear through the gate during injection molding, the smaller the Δb value. However, when the mass flow rate of the ethylene-propylene copolymer solution is too high, a spray state is formed at the gate, and the Δb value increases instead.
The ethylene-propylene copolymer has ethylene molar content in 9-15%, less vacuum holes and high light transmittance.
As can be seen from examples 1, 5, 14 and 15, the propylene butene copolymer has a melt flow rate of 5 to 15g/10min, less vacuum holes, smaller DeltaB number and a better freshness of the material. Within the above range, the higher the melt mass flow rate of the propylene-butene copolymer, the lower the shear through the gate during injection molding, the smaller the Δb value. However, when the melt mass flow rate of the propylene-butene copolymer is too high, a spray state is formed at the gate, and the Δb value increases instead.
As can be seen from examples 1, 6, 7, 10 and 11, the random copolymer polypropylene resin has a melt flow rate of 6 to 30g/10min, less vacuum holes, smaller DeltaB value, and a better freshness of the material. Within the above range, the higher the melt mass flow rate of the random copolymer polypropylene resin, the lower the shear through the gate during injection molding, and the smaller the Δb value. However, when the mass flow rate of the solution of the random copolymer polypropylene resin is too high, a spray state is formed at the gate, and the Δb value increases instead.
It can be found from examples 1, 16 and 17 that the beta-crystal form copper phthalocyanine blue is more favorable for reducing the color difference DeltaB between the injection-molded product and the raw material compared with other crystal forms copper phthalocyanine blue.
As can be seen from examples 1 and 18, the DeltaB value of the color plate can be rapidly reduced after the addition of an appropriate amount of the color difference regulator in example 1;
as can be seen from examples 1 and 19, the preferred stabilizer system used in example 1 has a high purity and contains little free phenol material because the antioxidant does not contain a phenol structure, and thus prevents extremely small amounts of phenol yellowing and/or quinone redness from occurring during high temperature injection molding, thus resulting in a rapid decrease in the DeltaB value.
As can be seen from examples 1 and 20, the use of the pre-grinding of the stabilizer and the color difference adjuster is advantageous in improving the freshness of the material.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.
Claims (10)
1. The polypropylene compound is characterized by comprising the following components in parts by weight:
60-96 parts of random copolymer polypropylene;
2-20 parts of ethylene propylene copolymer;
2-20 parts of propylene butene copolymer;
0.1-0.9 part of stabilizer;
0-0.05 part of color difference regulator;
in the random copolymer polypropylene, the mol content of ethylene is 1% -3.9%;
the ethylene propylene copolymer has ethylene mole content of 9% -16%;
in the propylene-butene copolymer, the molar content of butene is 5% -18%.
2. The polypropylene composite according to claim 1, wherein the melt mass flow rate of the random copolymer polypropylene is 0.2-44g/10min at 230 ℃ and 2.16kg, and the test standard is GB/T3682-2018.
3. The polypropylene composite according to claim 1, wherein the ethylene propylene copolymer has a melt mass flow rate of 1.2 to 100g/10min at 230 ℃ and 2.16kg, with a test standard of GB/T3682-2018.
4. The polypropylene composite of claim 1, wherein the ethylene propylene copolymer has an ethylene molar content of from 9% to 15% and a test standard of SH/T1800-2016.
5. The polypropylene composite of claim 1, wherein the propylene butene copolymer has a melt mass flow rate of 2.8 to 19.8g/10min at 230 ℃ and 2.16kg, with a test standard of GB/T3682-2018.
6. The polypropylene composite of claim 1, wherein the color difference modifier is beta crystal form copper phthalocyanine blue.
7. The polypropylene composite according to claim 1, wherein the stabilizer comprises an antioxidant and/or an ultraviolet absorber, the antioxidant is a hydroxylamine antioxidant and/or a phosphite antioxidant, and the ultraviolet absorber is a benzotriazole ultraviolet absorber.
8. The polypropylene composite according to claim 7, wherein the stabilizer comprises hydroxylamine antioxidants, phosphite antioxidants and benzotriazole ultraviolet absorbers in a mass ratio of (1-2): (1-2): 1.
9. the method for preparing the polypropylene compound according to any one of claims 1 to 8, comprising the steps of:
grinding stabilizer and color difference regulator, mixing with atactic copolymerized polypropylene, ethylene-propylene copolymer and propylene-butylene copolymer, adding into extruder, melt blending at 180-230 deg.c, extruding and pelletizing to obtain polypropylene composite.
10. Use of the polypropylene composite according to any one of claims 1 to 8 for the preparation of light-transmitting polypropylene injection molded articles.
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