CN114031847B - Modified polypropylene composite material with good appearance, high flatness and high filling performance, and preparation method and application thereof - Google Patents
Modified polypropylene composite material with good appearance, high flatness and high filling performance, and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/14—Copolymers of propene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/527—Cyclic esters
Abstract
The invention relates to a polypropylene composite material with good appearance, high flatness and high filling. The modified polypropylene composite material with good appearance, high flatness and high filling comprises pre-dispersed talcum powder master batch, talcum powder, dispersing agent and other processing aids. The modified polypropylene composite material provided by the invention can effectively improve the dispersion degree of talcum powder and the flow mark defect and warping degree during extrusion by selecting the nucleating agent master batch and carrying out dispersion treatment on the pre-dispersed talcum powder master batch, and the appearance pock and the flow mark defect of a finished product are effectively improved, and the flatness is high.
Description
Technical Field
The invention belongs to the field of modified plastics, and particularly relates to a modified polypropylene composite material with good appearance, high flatness and high filling, and a preparation method and application thereof.
Background
The talcum powder filling modified polypropylene product is commonly used in the fields of household appliances and automobiles, talcum powder is added into polypropylene, the rigidity and the surface hardness of the material can be improved, the dispersion difficulty of talcum powder is gradually improved along with the improvement of the adding amount of talcum powder, and the defects of surface pits, flow marks, evenness reduction and the like can occur particularly in extrusion-grade products.
Patent CN104403199a discloses a method for improving the dispersion of talc powder, which adopts superfine compressed talc powder and adds silicone master batch as a dispersing agent. Although this approach can improve the pitting defects of the extruded product at high loadings (27-45% talc content), it does not focus on how to improve the flow mark and flatness performance of the extruded product.
Therefore, the development of the modified polypropylene product which can improve the pock of the extruded product, can improve the flow mark and the flatness and is suitable for talcum powder high filling has important research significance and economic value.
Disclosure of Invention
The invention aims to overcome the defect or defect of poor flatness of talcum powder filled modified polypropylene products in the prior art and provides a modified polypropylene composite material with good appearance, high flatness and high filling. The modified polypropylene composite material provided by the invention can effectively improve the dispersion degree of talcum powder and the flow mark defect and warping degree during extrusion by selecting the nucleating agent master batch and carrying out dispersion treatment on the pre-dispersed talcum powder master batch, and the appearance pocky point and the flow mark defect of a finished product are effectively improved, and the flatness is high.
Another object of the present invention is to provide a method for preparing the above-mentioned modified polypropylene composite material with good appearance, high flatness and high filling.
The invention also aims to provide the application of the modified polypropylene composite material with good appearance, high flatness and high filling in the preparation of household appliances and automobile industry products.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the modified polypropylene composite material with good appearance, high flatness and high filling comprises the following components in parts by weight:
the pre-dispersed talcum powder master batch comprises the following components in parts by weight:
the nucleating agent master batch comprises the following components in parts by weight:
the inventor of the invention discovers that the crystallization degree and the isotacticity of matrix resin can be improved by preparing the polypropylene and the nucleating agent into the nucleating agent master batch, the cooling and shaping speed of a demolding head in the extrusion process of the modified polypropylene composite material can be increased, the flow mark defect can be effectively improved, the warping degree can be reduced, and the flatness can be improved.
In addition, the pre-dispersed talcum powder master batch is prepared by using the nucleating agent master batch, talcum powder and dispersing agent, and the dispersing degree of talcum powder can be effectively improved through multiple pre-dispersing, and the appearance pock defect of the finished product can be effectively improved.
The invention can effectively improve the dispersion degree of talcum powder, flow mark defect and warping degree during extrusion, and the appearance pock and flow mark defect of finished products are effectively improved, and the flatness is high through the selection of the nucleating agent master batch and the dispersion treatment of the pre-dispersed talcum powder master batch.
The crystallinity of polypropylene is determined by the following method: differential Scanning Calorimeter (DSC) method, reference: hou, physical and chemical examination-physical handbook, volume 43, 2007, 9.
The isotacticity of polypropylene is determined by the following method: infrared spectroscopy (IR), reference: li Cong, infrared spectroscopy in analysis of polypropylene isotacticity, guangzhou chemical industry, month 2, volume 41, phase 4.
Conventional polypropylene in the art may be used in the present invention.
Preferably, the polypropylene is one or more of homo-polypropylene and/or co-polypropylene.
Preferably, the polypropylene has a melt flow rate of 0.3-5 g/10min at 230 ℃ and 2.16kg according to GB/T3682-2018; more preferably 0.5 to 1.0/10min.
Preferably, the talc has an average particle diameter of 2 to 8. Mu.m.
Dispersants, nucleating agents conventional in the art may be used in the present invention.
Preferably, the dispersing agent is one or more of stearic acid dispersing agent, amide dispersing agent, ester dispersing agent or PPA fluorine dispersing agent.
More preferably, the stearic acid-based dispersant is one or both of calcium stearate or zinc stearate.
More preferably, the amide dispersant is one or more of erucamide, oleamide or ethylene distearate amide.
More preferably, the ester dispersant is a polyester polymeric dispersant, preferably Lu Bo wet produced ester dispersant such as DP310.
More preferably, the PPA fluorine-based dispersant is a PPA-based specialty fluoroelastomer copolymer, preferably a PPA-based product produced by U.S. 3M, such as FX-5920A, FX-5911, FX-5924, FX-5914X, FX-5922.
Preferably, the nucleating agent is one or more of benzoic acid nucleating agent, sorbitol nucleating agent or phosphate nucleating agent.
More preferably, the benzoic acid nucleating agent is one or more of sodium benzoate and lithium benzoate.
More preferably, the sorbitol nucleating agent is one or more of dibenzylidene alcohol (DBS), p-methylbenzylidene sorbitol (MDBS), di (p-chlorobenzylidene) sorbitol (CDBS) or di (p-ethylbenzylidene sorbitol) (EDBS).
More preferably, the phosphate nucleating agent is sodium 2,2' -methylene-bis (4, 6-di-tert-butylphenol) phosphate.
Preferably, the weight portion of the other processing aid is 0.1-2.5 portions, and the other processing aid is one or more of an antioxidant, a coupling agent or a weather-proof agent.
More preferably, the antioxidant is one or more of hindered phenol antioxidants, phosphite antioxidants, thioether antioxidants and hydroxylamine antioxidants.
More preferably, the coupling agent is one or two of N- (beta-aminoethyl) -gamma-aminopropyl trimethoxysilane or gamma-aminopropyl triethoxysilane.
More preferably, the weather-resistant agent is one or more of a Hindered Amine (HALS) light stabilizer or a benzophenone ultraviolet absorber.
It should be understood that the types and parts by weight of the nucleating agent masterbatch, the pre-dispersed talc masterbatch and other functional additives in the high-flatness high-filling extrusion-grade modified polypropylene composite material with good appearance are mutually independent.
Preferably, the nucleating agent master batch is prepared by the following steps: and uniformly mixing polypropylene, a nucleating agent, a dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the nucleating agent master batch.
Preferably, the pre-dispersed talcum powder master batch is prepared by the following steps: and uniformly mixing polypropylene, a nucleating agent master batch, talcum powder, a dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the pre-dispersed talcum powder master batch.
The preparation method of the modified polypropylene composite material with good appearance, high flatness and high filling is characterized by comprising the following steps: uniformly mixing the pre-dispersed talcum powder master batch, talcum powder, dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the modified polypropylene composite material with good appearance, high flatness and high filling.
Preferably, the conditions of the melt extrusion are: 180-200 ℃ in the first area, 180-200 ℃ in the second area, 190-220 ℃ in the third area, 220-240 ℃ in the fourth area, 220-240 ℃ in the fifth area, 220-240 ℃ in the sixth area, 220-240 ℃ in the seventh area, 220-240 ℃ in the eighth area, 200-230 ℃ in the ninth area and 250-360 revolutions per minute of the host machine.
Under the condition of melt extrusion, as the pre-dispersed talcum powder master batch is prepared in advance, the melt index stability of the finished product is good, and the current and torque stability in the extrusion process is better.
The application of the modified polypropylene composite material with good appearance, high flatness and high filling in the preparation of household appliances and automobile industry products is also within the protection scope of the invention.
Compared with the prior art, the invention has the following beneficial effects:
the modified polypropylene composite material provided by the invention can effectively improve the dispersion degree of talcum powder and the warping degree during extrusion by selecting the nucleating agent master batch and dispersing the pre-dispersed talcum powder master batch, and the finished product has effectively improved appearance pock and flow mark defects and high flatness.
Detailed Description
The invention is further illustrated below with reference to examples. These examples are only for illustrating the present invention and are not intended to limit the scope of the present invention. The experimental procedures in the examples below, without specific details, are generally performed under conditions conventional in the art or recommended by the manufacturer; the raw materials, reagents and the like used, unless otherwise specified, are those commercially available from conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art in light of the above teachings are intended to be within the scope of the invention as claimed.
The reagents selected for the examples and comparative examples of the present invention are described below:
polypropylene 1: homo-polypropylene, yanshan petrochemical B1101 and melt flow rate of 0.5g/10min;
polypropylene 2: copolymerized polypropylene, yanshan petrochemical B8101, and melt flow rate of 0.6g/10min;
polypropylene 3: homo-polypropylene, tianjin petrochemical T30S, and the melt flow rate is 3.0g/10min;
talcum powder 1: TYT-777A, the average grain size of the additive source of the factory sea city is 3.5 μm;
talcum powder 2: AH-1250N6, guangxi Ai Hai, manufacturer, with average particle size of 8.7 μm;
dispersant 1: PPA fluorine-based lubricants, commercially available;
dispersant 2: polyester polymer type dispersants, commercially available.
Nucleating agent 1: sorbitol nucleating agents, commercially available.
Nucleating agent 2: phosphate nucleating agents, commercially available.
An antioxidant: the main antioxidant and the auxiliary antioxidant are compounded according to the weight ratio of 1:1; and (3) a main antioxidant: 1010, commercially available; auxiliary antioxidant: 168, commercially available.
It should be understood that certain agents (e.g., dispersant 1, dispersant 2, nucleating agent 1, nucleating agent 2, antioxidant) selected in the examples and comparative examples are identical unless otherwise specified.
The formulation of the nucleating agent master batch is shown in table 1 and is prepared by the following steps: the components in Table 1 were mixed homogeneously and then fed from the main feed port of the extruder. The raw materials are melted, extruded and granulated in an extruder to obtain the nucleating agent master batch.
TABLE 1 formulation (parts) of nucleating agent masterbatch 1-5
The formulation of the pre-dispersed talc master batch is shown in Table 2 and is prepared by the following steps: the components in Table 2 were mixed homogeneously and then fed from the main feed port of the extruder. The raw materials are melted, extruded and granulated in an extruder to obtain the pre-dispersed talcum powder master batch.
TABLE 2 prescriptions (parts) of pre-dispersed talcum powder master batches 1-7
The modified polypropylene composite material in the embodiment and the comparative example is prepared by the following steps:
the raw materials of the embodiment and the comparative example are placed in a high-speed mixer to be evenly mixed, then the mixture is fed from a main feeding port of an extruder, and the raw materials are melted, extruded and granulated in the extruder to obtain the modified polypropylene composite material. Wherein, the temperature of the first area is 190 ℃, the temperature of the second area is 190 ℃, the temperature of the third area is 200 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the seventh area is 230 ℃, the temperature of the eighth area is 230 ℃, the temperature of the ninth area is 215 ℃, and the rotating speed of the host machine is 300 revolutions per minute.
The modified polypropylene composite materials of the examples and comparative examples of the present invention were tested as follows:
(1) Tensile strength: GB/T1040.2-2006.
(2) Elongation at break: GB/T1040.2-2006.
(3) Cantilever impact strength (a notch): GB/T1843-2008.
(4) Flexural strength: GB/T9341-2008.
(5) Flexural modulus: GB/T9341-2008.
(6) Extruded article appearance: extruding 50cm×50cm×5mm product, observing surface flow mark and pit number: the number of flow marks is 2, the number of flow marks is 2-5, the number of flow marks is B, and the number of flow marks is >5, the number of flow marks is C; the number of pits <2 is class A, the number of pits 2-10, (including 2 and including 10) is class B, the number of pits 10-50 (excluding 10 and including 50) is class C, and the number of pits >50 is class D.
(7) 50 cm. Times.50 cm. Times.5 mm extruded article warp height: the maximum warp height for each corner was recorded by direct measurement.
(8) Current/torque stability during extrusion: the current/torque during extrusion was recorded per hour, the variance was calculated with <2 being class a, variance 2-3 (including 2 excluding 3) being class B and variance 3-5 (including 3 excluding 5) being class C.
Examples 1 to 10
This example provides a series of good appearance, high flatness, high fill modified polypropylene composites with the formulations shown in Table 3.
Table 3 formulations (parts) of examples 1 to 10
Comparative examples 1 to 2
This comparative example provides a series of polypropylene alloy compositions.
The amounts of the components used in comparative examples 1 and 2 were the same as in example 1, but the nucleating agent masterbatch 1 and the pre-dispersed talc masterbatch 1 were not prepared in advance in comparative example 1, but the components were directly mixed and melted, extrusion granulated. In comparative example 2, the nucleating agent masterbatch 1 was prepared in advance, but the pre-dispersed talc masterbatch 1 was not prepared in advance, but the components were directly mixed and melt, extrusion granulated.
The modified polypropylene composites provided in each example and comparative example were tested for properties according to the performance test methods described above, and the results are shown in Table 4.
Table 4 results of Performance test of the Polypropylene alloy compositions provided in examples 1 to 10 and comparative examples 1 to 2
From the above test results, it can be seen that the modified polypropylene composite materials with good appearance, high flatness and high filling provided in examples 1 to 10 have significantly improved pocking marks and flow mark defects under the high filling of talcum powder, and have high flatness, better mechanical properties, and good current/torque stability during extrusion process, so that the overall performance of example 1 is optimal. The comparative example 1 was obtained by directly mixing the respective raw materials, and had defects of pitting and flow marks, poor flatness, poor mechanical properties, and poor current/torque stability during extrusion. Although the nucleating agent master batch prepared in comparative example 2 is favorable for improving the crystallinity and isotacticity of matrix resin, accelerating the cooling and shaping speed of a die head in the extrusion process of the modified polypropylene composite material, further improving the mechanical property, improving flow marks to a certain extent and reducing warping, the talcum powder has still poor dispersibility and has the defect of pitting.
Those of ordinary skill in the art will recognize that the embodiments herein are intended to assist the reader in understanding the principles of the invention and should be understood that the scope of the invention is not limited to such specific statements and embodiments. Those of ordinary skill in the art can make various other specific modifications and combinations from the teachings of the present disclosure without departing from the spirit thereof, and such modifications and combinations remain within the scope of the present disclosure.
Claims (6)
1. The modified polypropylene composite material with good appearance, high flatness and high filling is characterized by comprising the following components in parts by weight:
66.5 to 79.7 parts of pre-dispersed talcum powder master batch,
18-30 parts of talcum powder,
0.2-1 part of a dispersing agent,
0-2.5 parts of other processing aids;
the pre-dispersed talcum powder master batch comprises the following components in parts by weight:
63.5-74.7 parts of polypropylene,
3-5 parts of a nucleating agent master batch,
20-32 parts of talcum powder,
0.2-1 part of a dispersing agent,
0-2.5 parts of other processing aids;
the nucleating agent master batch comprises the following components in parts by weight:
87.5-89.9 parts of polypropylene,
10-18 parts of a nucleating agent,
0 to 0.5 part of a dispersing agent,
0-2.5 parts of other processing aids;
the polypropylene is homo-polypropylene and/or co-polypropylene; the melt flow rate of the polypropylene at 230 ℃ and 2.16kg is 0.3-5 g/10min according to GB/T3682-2018;
the average particle size of the talcum powder is 2-8 mu m;
the dispersing agent is one or more of polyester high molecular dispersing agent or PPA fluorine dispersing agent;
the nucleating agent is one or more of sorbitol nucleating agent and phosphate nucleating agent.
2. The modified polypropylene composite material with good appearance and high flatness and filling according to claim 1, wherein the weight parts of the other processing aids are 0.1-2.5 parts; the other processing aid is one or more of an antioxidant, a coupling agent or a weather-proof agent.
3. The modified polypropylene composite material with good appearance and high flatness and filling according to claim 1, wherein the nucleating agent master batch is prepared by the following steps: and uniformly mixing polypropylene, a nucleating agent, a dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the nucleating agent master batch.
4. The modified polypropylene composite material with good appearance and high flatness and filling according to claim 1, wherein the pre-dispersed talcum powder master batch is prepared by the following steps: and uniformly mixing polypropylene, a nucleating agent master batch, talcum powder, a dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the pre-dispersed talcum powder master batch.
5. The method for preparing the modified polypropylene composite material with good appearance, high flatness and high filling in any one of claims 1 to 4, which is characterized by comprising the following steps: uniformly mixing the pre-dispersed talcum powder master batch, talcum powder, dispersing agent and other processing aids to obtain a mixture, and then carrying out melt extrusion and granulation on the mixture to obtain the modified polypropylene composite material with good appearance, high flatness and high filling.
6. The use of the modified polypropylene composite material with good appearance, high flatness and high filling in any one of claims 1-4 for preparing products in household appliances and automobile industry.
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| 李伟 ; 陈嘉杰 ; 胡佳旭 ; 赖昂 ; 雷亮 ; 吴国峰 ; 俞飞 ; 杨波 ; 罗忠富 ; .POE黏度和含量对PP及其填充体系性能的影响.工程塑料应用.2020,(10),全文. * |
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| CN114031847A (en) | 2022-02-11 |
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