WO2018107950A1 - 一种消除聚丙烯组合物虎皮纹缺陷的方法及其制备的聚丙烯组合物 - Google Patents

一种消除聚丙烯组合物虎皮纹缺陷的方法及其制备的聚丙烯组合物 Download PDF

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Publication number
WO2018107950A1
WO2018107950A1 PCT/CN2017/112492 CN2017112492W WO2018107950A1 WO 2018107950 A1 WO2018107950 A1 WO 2018107950A1 CN 2017112492 W CN2017112492 W CN 2017112492W WO 2018107950 A1 WO2018107950 A1 WO 2018107950A1
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Prior art keywords
polypropylene composition
polypropylene
tiger skin
screw
composition according
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PCT/CN2017/112492
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English (en)
French (fr)
Inventor
李振华
李伟
杨波
吴国峰
罗忠富
王琪
苏娟霞
蒋团辉
雷亮
Original Assignee
金发科技股份有限公司
天津金发新材料有限公司
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Publication of WO2018107950A1 publication Critical patent/WO2018107950A1/zh

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • 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
    • B29C48/50—Details of extruders
    • B29C48/505—Screws
    • 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
    • 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
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • 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
    • B29C2948/9258—Velocity
    • B29C2948/926—Flow or feed rate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the invention relates to the technical field of polymer material polypropylene, in particular to a polypropylene composition for eliminating tiger skin defect and a preparation method thereof.
  • Polypropylene PP a semi-crystalline plastic with low density and easy processing, is widely used in car bumpers and interiors.
  • the polypropylene material is prone to defects in the appearance of the tiger skin, which affects the appearance of the part and the subsequent processing performance.
  • CN102964686A uses a small molecular polypropylene with a flow rate of 1800 g/10 min as a tiger skin grain remover to prepare a composite material for eliminating tiger skin texture, and briefly describes the preparation method.
  • CN104558834A discloses a good injection molding grade high performance polypropylene composite material and a preparation method thereof, which are compounded with high flow property polypropylene (40-100 g/min) and low flow (0.5-5 g/min) polypropylene. The molecular weight distribution of the material is improved, and a polypropylene composite material excellent in mechanical properties is obtained.
  • the above materials have hardly seen industrial production schemes, and there are many uncertain factors in the industrial production process. Therefore, it is necessary to study the stable preparation process of the polypropylene composition for eliminating tiger skin defects.
  • the object of the present invention is to overcome the deficiencies of the prior art and to provide a stable preparation method for a polypropylene composition which eliminates tiger skin defect.
  • Another object of the invention is to provide a polypropylene composition prepared by the process.
  • a method for preparing a polypropylene composition for eliminating tiger skin defects comprising the steps of:
  • the raw materials of the polypropylene composition are uniformly mixed and then added to a twin-screw extruder;
  • the mixture is melt-kneaded, and the temperature of each section of the extruder is the same, 190-200 ° C, and the screw rotation speed is 400-600 rpm;
  • the polypropylene composition raw material in the step S1 comprises the following parts by weight:
  • the polypropylene resin is prepared by the following components in mass percentage:
  • the screw combination sequence of the melt plasticizing section of the twin-screw extruder in step S2 is 45/5/42, 45/5/42, 36/36, 45/5/42, 45/5/42, 36/ 36, 45/5/42, 45/5/42, 45/5/42 L
  • the screw combination sequence of the mixed dispersion section is 45/5/42, 45/5/42, 45/5/42, 52/52 45/5/42, 45/5/42, 45/5/42, 52/52, 36/36, 45/5/42, 45/5/42, 45/5/42.
  • the threaded elements in the extruder screw combination comprise a conveying element and a shearing element.
  • the type of conveying element is mainly divided from the lead (the axial length around one turn) and the length of the component (the axial length of the element).
  • 72/36 can represent the conveying element
  • 72 is the guiding process
  • 36 is the length of the component. , in millimeters.
  • the models mainly include 96/96, 72/72, 56/56, 72/32, 56/28, and 72/36L (L refers to the left direction, generally not indicated in the forward direction), 56/28L, and the like.
  • the shearing element is the engaging block, which is meshed together by a single cutting block.
  • the twin-screw extruder of the invention comprises a blank conveying section, a melt plasticizing section, a mixing and dispersing section, a vacuum exhaust section and an extrusion building section, wherein the screw combination of the melt plasticizing section and the mixing dispersion section is a polypropylene combination
  • the tiger skin defect of the object has an effect.
  • the invention applies different screw combinations in the melt plasticizing section and the mixing dispersion section of the extruder screw, and the shearing is more uniform by the design of the screw combination, so that the material can be effectively dispersed while reducing the shearing, so that the components are The rubber phase particles are as large as possible and evenly dispersed.
  • the mutual integration can eliminate the tiger skin pattern produced by the material in the injection molding process and improve the stability of industrial production.
  • the toughening agent in the raw material of the polypropylene composition refers to a toughening agent commonly used in the prior art.
  • the toughening agent is an ethylene-butene copolymer and/or an ethylene-octene copolymer.
  • the toughening agent has a density of 0.85 to 0.87 g/cm 3 , a Tg ⁇ -50 ° C, and a melt flow rate of 0.1 to 2 g/10 min at 190 ° C ⁇ 2.16 kg.
  • the filler refers to a filler commonly used in the prior art, and specifically may be one or two of talc, calcium carbonate, wollastonite, whiskers or glass fibers.
  • the auxiliary agent refers to an auxiliary agent commonly used in the prior art, and specifically may be an antioxidant, a light stabilizer, a lubricant, and a nucleating agent.
  • the antioxidant is a hindered phenol or phosphite antioxidant, specifically one of the types 1010, 1076, 3114, 168, PEP-36 or a mixture of two or more.
  • the light stabilizer is a hindered amine light stabilizer, specifically one of the models UV-3808PP5, LA-402XP, LA-402AF or a mixture of two or more.
  • the present invention has the following beneficial effects:
  • the high flow resin is compounded with the low flow resin, and the dispersion of the two different fluid materials has a relatively large problem, especially in the industrial production process, the stability is difficult to be guaranteed.
  • the invention adopts the design of the screw combination to make the shearing more uniform, so that the material can reduce the shear while effectively dispersing, so that the rubber phase particles in the component are as large as possible, the degree of the amorphous shape is as large as possible and the distribution is uniform.
  • the prepared polypropylene composition can be used in automotive bumpers and interior products.
  • the polypropylene PP1 used is a high-flow polypropylene resin supplied by Total, at a temperature of 230 ° C ⁇ 2.16 kg, a melt flow rate of 60-120 g/10 min;
  • PP2 is a commercially available PP resin as a low-flow polypropylene resin.
  • the supplier is Basel, and the melt flow rate is 1-10 g/10 min at 230 ° C ⁇ 2.16 kg.
  • the toughening agent selected in the present invention is POE, commercially available, having a density of 0.85 to 0.87 g/cm 3 , Tg ⁇ -50 ° C, and a melt flow rate of 0.1 to 2 g/10 min under the condition of 190 ° C ⁇ 2.16 kg.
  • the filler of the present invention is selected from talc powder, and the pigment is selected from carbon black;
  • the auxiliary agent is selected from antioxidants, light stabilizers, lubricants and nucleating agents commonly used in the prior art.
  • the antioxidant of the invention is selected from the antioxidants 1010 and 168, the light stabilizer is selected as the model UV-3808PP5, the lubricant is selected as the TR-451, and the nucleating agent is selected as the HPN- 20E.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 200 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 200 ° C
  • the screw rotation speed was 600 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • Squeeze The temperature of each section of the outlet was 200 ° C, the screw rotation speed was 400 rpm, and extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 200 ° C
  • the screw rotation speed was 600 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed according to the ratio of Table 1, and then added to the twin-screw extruder, and the screw combination 2 was selected for melt-kneading, that is, the screw combination order of the melt plasticizing section of the extruder was 45/5/42.
  • the screw combination order of the mixed dispersion section is 45/5/42, 90/5/42, 45/5/27, 45/5/27 L, 52/52, 36/36, 45/5/42, 90/5/42, 45/5/27, 45/5/27 L, 52/52, 52/52, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed according to the ratio of Table 1, and then added to the twin-screw extruder, and the screw combination 3 was selected for melt-kneading, that is, the screw combination order of the melt plasticizing section of the extruder was 45/5/42.
  • the screw combination order of the mixed dispersion section is 45/5/42, 90/5/42, 45/5/42 L, 52/52, 45/5/42, 45/5/42, 45/5/42 L, 52/52, 36/36, 45/5/42, 45/5/42 L.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 800 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the screw combination sequence is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/36, 45/5/42, 45/5/42, 45/ 5/42.
  • the temperature of each section of the extruder was 210 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the raw materials of the polypropylene composition were uniformly mixed and then added to a twin-screw extruder, and the screw combination 1 was selected for melt-kneading, that is, the screw combination sequence of the melt plasticizing section of the extruder was 45/5/42.
  • the order of screw combination is 45/5/42, 45/5/42, 45/5/42, 52/52, 45/5/42, 45/5/42, 45/5/42, 52/52, 36/ 36, 45/5/42, 45/5/42, 45/5/42.
  • the temperature of each section of the extruder was 190 ° C
  • the screw rotation speed was 400 rpm
  • extrusion granulation was carried out to obtain a polypropylene composition.
  • the prepared polypropylene composition was injected into the mechanical spline for testing the notched impact strength and flexural modulus of the simply supported beam.
  • the injection long rectangular plate was used to evaluate the tiger skin effect, and the tiger skin effect was smooth with 108*328 mm.
  • the flat panel is evaluated, preferably 1 level, and the worst level is 5 levels, which are scored by 3-5 reviewers and evaluated.
  • the process stability test the same raw materials were used to prepare a polypropylene composition under the same preparation process, and a rectangular long plate was injection-molded to evaluate the tiger skin effect.
  • Notched beam notched impact strength tested in accordance with ASTM D256;
  • flexural modulus tested in accordance with ASTM D790;
  • melt flow rate (melt) ASTM D1238.
  • the increase in the proportion of the high-flowing resin PP1 in the combined system can increase the rigidity (bending modulus) and tensile strength of the material, but the molecular chain entanglement of the high-flowing polymer decreases, and the tensile force between the molecular chains decreases.
  • the impact strength is lowered; the increase in the PP2 component results in an increase in impact strength, a decrease in rigidity (bending modulus) and tensile strength, and a deterioration in melt flow properties.
  • the mechanical properties exhibited by different processes under the same formulation conditions will also vary, and the same formulation will have performance differences under the same process, which will be related to the injection quality of the test splines and the normal error of the test system.
  • the screw combination 1 is a combination of a thread element having a weak overall shear strength, and the material can be more uniformly sheared than the screw combination 2 having a moderate overall shear strength and the screw combination 3 having a higher overall shear strength. Allowing the material to reduce shear while effectively dispersing, so that the rubber phase particles in the component are as large as possible, and the high flow resin and rubber When the system is pulled together, there will be no high flow zone and low flow zone in the whole melt system, in order to reduce the uneven flow of materials in the process of subsequent material injection, and increase the mutual fusion between different material combinations, which can eliminate materials.
  • the tiger skin pattern produced during the injection molding process enhances the stability of industrial production. From the results of Table 3, the preparation method of the present invention has high process stability, and the polypropylene composition is prepared by this method 6 times, and the tiger skin texture effect is 1 level.

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Abstract

本发明公开了一种消除虎皮纹缺陷聚丙烯组合物的制备方法及制备的聚丙烯组合物。所述聚丙烯组合物包括聚丙烯树脂、增韧剂、填料、颜料、助剂，其中，所述聚丙烯树脂采用熔体质量流动速率(MFR)为30～120g/10min的高流动聚丙烯和熔体质量流动速率(MFR)为0.1～29g/10min的低流动聚丙烯进行复配。制备方法通过螺杆组合设计以及挤出工艺参数调整使得制备的聚丙烯组合物能够消除虎皮纹，且制备工艺稳定，可重复性好。本发明所制备的聚丙烯组合物可以用于汽车保险杠以及内饰产品中。

Description

一种消除聚丙烯组合物虎皮纹缺陷的方法及其制备的聚丙烯组合物 技术领域
本发明涉及高分子材料聚丙烯技术领域，尤其涉及一种消除虎皮纹缺陷的聚丙烯组合物及其制备方法。
背景技术
聚丙烯PP，半结晶性塑料，具有密度低、易加工等特点，在车用保险杠以及内饰中大量使用。然而聚丙烯材料在注塑过程中极易产生虎皮纹的外观缺陷，影响制件的外观效果以及后续的加工性能。
为了降低材料在注塑过程中产生的虎皮纹缺陷。CN102964686A采用一种流动速率为1800g/10min的小分子聚丙烯作为虎皮纹消除剂，制备一种消除虎皮纹的复合材料，并对制备方法做了简单阐述。CN104558834A公开了一种良好注塑级高性能聚丙烯复合材料及其制备方法，其采用高流动性能聚丙烯(40-100g/min)与低流动(0.5-5g/min)性能的聚丙烯进行复配，提升材料的分子量分布，得出机械性能优异的聚丙烯复合材料。然而上述材料几乎没有见到工业化生产方案，工业化生产过程中存在较多不确定性因素，因此对于消除虎皮纹缺陷的聚丙烯组合物的稳定制备工艺需要有一定研究。
发明内容
本发明的目的是克服现有技术存在的不足，提供一种消除虎皮纹缺陷的聚丙烯组合物的稳定制备方法。
本发明的另一目的在于提供一种由所述方法制备的聚丙烯组合物。
本发明的上述目的通过以下技术方案予以实现：
一种消除虎皮纹缺陷聚丙烯组合物的制备方法，包括以下步骤：
S1.将聚丙烯组合物的原料混合均匀后加入双螺杆挤出机中；
S2.对上述混合物进行熔融混炼，挤出机各段温度相同，为190～200℃，螺杆转速为400～600转/分；
S3.挤出造粒；
步骤S1中所述聚丙烯组合物原料包括以下重量份：
聚丙烯树脂50～100份；
增韧剂10～30份；
填料0～20份；
颜料0～2份；
助剂0～2份；
其中，所述聚丙烯树脂由以下按质量百分比计的组分复配制得:
230℃×2.16kg条件下，熔体流动速率为30～120g/10min的高流动聚丙烯，70％～90％；
230℃×2.16kg条件下，熔体流动速率为0.1～29g/10min的低流动聚丙烯，10％～30％；
步骤S2中所述双螺杆挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。
挤出机螺杆组合中的螺纹元件包含输送元件和剪切元件。输送元件种类主要是从导程(绕一圈的轴向长度)和元件长度(元件轴向长度)来分，如72/36就可以代表这种输送元件，72是指导程，36是元件长度，单位毫米。型号主要有96/96、72/72、56/56、72/32、56/28、72/36L(L指左向，一般正向的不标明)、56/28L等。剪切元件就是啮合块,由单个的剪切块啮合在一起，片数不定，一般4-7片，单片厚度不一。主要是以各单片啮合的角度来确定规格型号，同样也分正反，可根据实际情况进行微调组合。剪切块型号举例:45/5/56L中，45指啮合角度45度，5是片数，56是长度，L指左向，特殊的剪切元件有齿型盘、拉伸流块。从螺杆组合整体效果看，单个的元件效果体现不明显，一般需要在特定的临近组合条件下才会有其真实的体现。
本发明的双螺杆挤出机包括下料输送段、熔融塑化段、混合分散段、真空排气段和挤出建压段，其中熔融塑化段和混合分散段的螺杆组合对聚丙烯组合物的虎皮纹缺陷有影响。本发明通过在挤出机螺杆的熔融塑化段和混合分散段加载不同的螺杆组合，通过螺杆组合的设计，剪切更加均匀，使得物料能够在有效分散的同时降低剪切，使得组分中的橡胶相颗粒尽可能的大，且分散均匀。这样可将高流动树脂与橡胶体系拉在一起，整个熔体体系里面不会出现高流动区和低流动区，才能在后续物料注塑的过程中通过减少物料的不均匀流动，增加不同物料组合之间的互相融合，能够消除物料在注塑过程中产生的虎皮纹，提升工业生产的稳定程度。
所述聚丙烯组合物原料中增韧剂是指现有技术常用的增韧剂，优选地，所述增韧剂为乙烯-丁烯共聚物和/或乙烯-辛烯共聚物。
优选地，所述增韧剂密度为0.85～0.87g/cm3，Tg≤-50℃，190℃×2.16kg条件下熔体 流动速率为0.1～2g/10min。
所述填料是指现有技术常用的填料，具体可以为滑石粉、碳酸钙、硅灰石、晶须或玻璃纤维中的一种或两种。
所述颜料是指现有技术常用的填料，具体可为炭黑。
所述助剂是指现有技术常用的助剂，具体可为抗氧剂、光稳定剂、润滑剂、成核剂。
所述抗氧剂为受阻酚类或亚磷酸酯类抗氧剂，具体可以是型号1010、1076、3114、168、PEP-36中的一种或者两种及以上的混合物。
所述光稳定剂为受阻胺类光稳定剂，具体可以是型号UV-3808PP5、LA-402XP、LA-402AF中的一种或者两种及以上的混合物。
所述润滑剂是指现有技术常用的润滑剂，具体为硅酮类、酯类、酰胺类、聚乙烯类、硬脂酸类、脂肪酸及酯类中的一种或者两种及以上的混合物。
与现有技术相比，本发明具有如下有益效果：
高流动树脂与低流动树脂复配，两种不同流动性的物料相间的分散存在比较大的问题，特别在工业化生产过程中，稳定性难以得到保证。本发明通过螺杆组合的设计，剪切更加均匀，使得物料能够在有效分散的同时降低剪切，使得组分中的橡胶相颗粒尽可能的大，不定形程度尽可能的大且分布均匀，才能在后续物料注塑的过程中通过减少物料的不均匀流动，增加不同物料组合之间的互相融合，能够消除物料在注塑过程中产生的虎皮纹，提升工业生产的稳定程度。所制备的聚丙烯组合物可以用于汽车保险杠以及内饰产品中。
具体实施方式
下面结合具体实施例对本发明进行进一步解释说明，以下实施例为本发明较佳的实施方式，但本发明的实施方式并不受下述实施例的限制。但凡采用等同替换或等效变换的形式所获得的技术方案，均应包括在本发明权利要求的保护范围之内。
采用的聚丙烯PP1为高流动聚丙烯树脂，供应商为道达尔，230℃×2.16kg条件下，熔体流动速率为60-120g/10min；PP2为市售PP树脂为低流动聚丙烯树脂，供应商为巴塞尔，230℃×2.16kg条件下，熔体流动速率为1-10g/10min。
本发明选用的增韧剂为POE，市售，密度为0.85～0.87g/cm3，Tg≤-50℃，190℃×2.16kg条件下熔体流动速率为0.1～2g/10min。
填料、颜料为本领域现有技术常用的型号，本发明填料选用滑石粉，颜料选用炭黑；助剂选用本领域现有技术常用的抗氧剂、光稳定剂、润滑剂、成核剂，本发明抗氧剂选用抗氧剂1010、168，光稳定剂选用型号UV-3808PP5，润滑剂选用TR-451，成核剂选用HPN- 20E。
实施例1
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
实施例2
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为200℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
实施例3
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为200℃，螺杆转速为600转/分，挤出造粒，得到聚丙烯组合物。
实施例4
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
实施例5
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤 出机各段温度为200℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
实施例6
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为200℃，螺杆转速为600转/分，挤出造粒，得到聚丙烯组合物。
对比例1
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合2进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、90/5/42、45/5/27、45/5/27 L，混合分散段的螺杆组合顺序为45/5/42、90/5/42、45/5/27、45/5/27 L、52/52、36/36、45/5/42、90/5/42、45/5/27、45/5/27 L、52/52、52/52、52/52、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
对比例2
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合3进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、90/5/42、36/36、45/5/42、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、90/5/42、45/5/42 L、52/52、45/5/42、45/5/42、45/5/42 L、52/52、36/36、45/5/42、45/5/42 L。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
对比例3
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为800转/分，挤出造粒，得到聚丙烯组合物。
对比例4
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、 45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为210℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
对比例5
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
对比例6
按表1配比将聚丙烯组合物原料混合均匀后加入双螺杆挤出机中，选用螺杆组合1进行熔融混炼，即挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42 L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。挤出机各段温度为190℃，螺杆转速为400转/分，挤出造粒，得到聚丙烯组合物。
性能评价方式及实行标准：
将制备的聚丙烯组合物注塑力学样条，用于测试其简支梁缺口冲击强度和弯曲模量；同时注塑矩形长板用于评估虎皮纹效果，虎皮纹效果采用108*328mm的光滑平板进行评估，最好为1级，最差为5级，由3-5名评测者分别打分并汇总评估。工艺稳定性测试，将相同的原料在同一个制备工艺下制备聚丙烯组合物，注塑矩形长板进行虎皮纹效果评级。
(1)简支梁缺口冲击强度：按照ASTM D256测试；(2)弯曲模量：按照ASTM D790测试；(3)融体流动速率(融指)，ASTM D1238。
测试得到的性能参数如表2、表3所示。
表1实施例和对比例的聚丙烯组合物的配方及制备方法
Figure PCTCN2017112492-appb-000001
表2实施例和对比例的聚丙烯组合物的性能测试
Figure PCTCN2017112492-appb-000002
表3工艺稳定性测试
Figure PCTCN2017112492-appb-000003
由表2中测试结果可得出：与实施例1相比，对比例1、2采用的螺杆组合2和3不能有效消除虎皮纹，力学性能也有所下降，螺杆组合1能够明显消除虎皮纹；对比例3与实施例1相比，通过转速的变化可以看出，转速升高造成虎皮纹缺陷严重。对比例4与实施例1相比，温度高于200℃后，虎皮纹缺陷不能消除。对比例5和对比例6与实施例1相比，仅采用低流动聚丙烯或高流动聚丙烯，不能完全消除虎皮纹。
物理性能方面，高流动树脂PP1在组合体系中的比例增加能够提升物料的刚性(弯曲模量)和拉伸强度，但是由于高流动聚合物的分子链缠绕变少，分子链间的拉力减小，使得其冲击强度会降低；PP2组分的含量增大会导致冲击强度增大，刚性(弯曲模量)和拉伸强度降低，同时熔体流动性能也变差。同样配方条件下的不同工艺呈现的力学性能也会有差异，而同样配方在相同工艺下会有性能差异，这些会与测试样条的注塑质量以及测试系统的正常误差相关。
实施例中螺杆组合1为整体剪切强度较弱的螺纹元件组合，相较于整体剪切强度适中的螺杆组合2和整体剪切强度较高的螺杆组合3，能够更加均匀的剪切物料，使得物料能够在有效分散的同时降低剪切，使得组分中的橡胶相颗粒尽可能的大，将高流动树脂与橡胶 体系拉在一起，整个熔体体系里面不会出现高流动区和低流动区，才能在后续物料注塑的过程中通过减少物料的不均匀流动，增加不同物料组合之间的互相融合，能够消除物料在注塑过程中产生的虎皮纹，提升工业生产的稳定程度。从表3结果来看，本发明制备方法工艺稳定性高，用此法6次制备聚丙烯组合物，虎皮纹效果均为1级。

Claims (10)

  1. 一种消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，包括以下步骤：
    S1.将聚丙烯组合物的原料混合均匀后加入双螺杆挤出机中；
    S2.对上述混合物进行熔融混炼，挤出机各段温度相同，为190～200℃，螺杆转速为400～600转/分；
    S3.挤出造粒；
    步骤S1中所述聚丙烯组合物原料包括以下重量份：
    聚丙烯树脂50～100份；
    增韧剂10～30份；
    填料0～20份；
    颜料0～2份；
    助剂0～2份；
    其中，所述聚丙烯树脂由以下按质量百分比计的组分复配制得:
    230℃×2.16kg条件下，熔体流动速率为30～120g/10min的高流动聚丙烯，70％～90％；
    230℃×2.16kg条件下，熔体流动速率为0.1～29g/10min的低流动聚丙烯，10％～30％；
    步骤S2中所述双螺杆挤出机的熔融塑化段的螺杆组合顺序为45/5/42、45/5/42、36/36、45/5/42、45/5/42、36/36、45/5/42、45/5/42、45/5/42L，混合分散段的螺杆组合顺序为45/5/42、45/5/42、45/5/42、52/52、45/5/42、45/5/42、45/5/42、52/52、36/36、45/5/42、45/5/42、45/5/42。
  2. 根据权利要求1所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述增韧剂为乙烯-丁烯共聚物和/或乙烯-辛烯共聚物。
  3. 根据权利要求2所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述增韧剂密度为0.85～0.87g/cm3，Tg≤-50℃，190℃×2.16kg条件下熔体流动速率为0.1～2g/10min。
  4. 根据权利要求1所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述填料为滑石粉、碳酸钙、硅灰石、晶须、玻璃纤维中的一种或两种以上。
  5. 根据权利要求1所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述颜料为炭黑。
  6. 根据权利要求1所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述助剂为抗氧剂、光稳定剂、润滑剂、成核剂。
  7. 根据权利要求6所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述抗氧剂为受阻酚类或亚磷酸酯类抗氧剂。
  8. 根据权利要求6所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述光稳定剂为受阻胺类光稳定剂。
  9. 根据权利要求6所述消除虎皮纹缺陷聚丙烯组合物的制备方法，其特征在于，所述润滑剂为硅酮类、酯类、酰胺类、聚乙烯类、硬脂酸类、脂肪酸及酯类中的一种或两种以上。
  10. 一种如权利要求1所述的方法制备的消除虎皮纹缺陷聚丙烯组合物。
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