CN108192213B - Polypropylene composite material and preparation method thereof - Google Patents
Polypropylene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polypropylene composite material and a preparation method thereof, belonging to the technical field of modified materials. The polypropylene composite material comprises the following components in parts by weight: 65-80 parts of polypropylene, 2-12 parts of tungsten disulfide nanorods and 1-8 parts of compatilizer. The invention uses specific content of tungsten disulfideThe nano-rod is added into the polypropylene matrix under the synergistic dispersion effect of the compatilizer with specific content, so that WS in the prepared polypropylene composite material2Rub against each other to produce laminar sliding, WS2The friction is thinned and ground small, and small fragments fill the defects in the abrasion process, so that the friction fluctuation is further reduced, and the friction stability is enhanced. Therefore, the scratch resistance and the strength of the polypropylene composite material obtained by the invention are obviously improved.
Description
Technical Field
The invention relates to a polypropylene composite material and a preparation method thereof, belonging to the technical field of modified materials.
Background
The polypropylene is widely used in the industries of automobiles, household electrical appliances, packaging, pipes and the like due to light weight and low price, but has the defects of low surface hardness, higher friction coefficient, strength, low hardness, low surface polarity, easy scratching and the like. The use is limited, and the polypropylene is modified according to the use requirement to meet the use requirement in different fields.
The currently used methods are to add elastomer materials into a polypropylene matrix to improve the impact strength, to introduce 10-40% of fillers such as talcum powder, mica powder, wollastonite, kaolin and the like to improve the tensile strength, the bending strength and the bending modulus, and to introduce scratch-resistant agents such as silicone master batches and amide-containing resins to improve the scratch resistance. While such methods adjust the overall properties by simultaneously applying the elastomer, filler and scratch resistance, it is not easy to simultaneously achieve a balance of properties. The nano filler has the characteristics of large specific surface area, small size effect, surface interface effect and the like which are not possessed by micron-sized fillers, and the characteristics can realize synchronous reinforcement and toughening of the polymer composite material, improve the surface hardness of the material and show excellent scratch resistance. Prior art studies have found WS by activation treatment with silane coupling agent2Compounded with UHMWPE (ultra-high molecular weight polyethylene) to form UHMWPE (ultra-high molecular weight polyethylene)/nano WS2The preparation of the composite resin can improve the strength of UHMWPE (ultra-high molecular weight polyethylene) (Martian et al, preparation and performance of nano tungsten disulfide reinforced ultra-high molecular weight polyethylene novel bulletproof material. science report 2012.3329-3333), but the paper does not mention WS2The composite effect with polypropylene. Chinese patent CN105315418A mentions a preparation method of tungsten dioxide modified phenolic resin, wherein tungsten dioxide improves the corrosion resistance, wear resistance and the like of the phenolic resin, but the preparation method is complex, the preparation period is long, and mass production is not easy to realize.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a polypropylene composite material with surface scratch resistance and excellent mechanical property and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a polypropylene composite material comprises the following components in parts by weight: 65-80 parts of polypropylene, 2-12 parts of tungsten disulfide nanorods and 1-8 parts of compatilizer.
The tungsten disulfide nanorod is a compound of tungsten and sulfur, and the chemical formula of the tungsten disulfide nanorod is WS2(ii) a The compatilizer is an assistant for promoting two incompatible polymers to be combined into a whole by virtue of intermolecular bonding force, so as to obtain a stable blend.
According to the invention, tungsten disulfide nano rods with specific content are added into a polypropylene matrix under the synergistic dispersion effect of compatilizer with specific content, so that WS in the prepared polypropylene composite material2Rub against each other to produce laminar sliding, WS2The friction is thinned and ground small, and small fragments fill the defects in the abrasion process, so that the friction fluctuation is further reduced, and the friction stability is enhanced. Therefore, the scratch resistance and the strength of the polypropylene composite material obtained by the invention are obviously improved.
As a preferred embodiment of the polypropylene composite material, the tungsten disulfide nanorods are 7.5-10 parts by weight, and the compatilizer is 5-8 parts by weight. As a more preferable embodiment of the polypropylene composite material, the tungsten disulfide nano-rods account for 10 parts by weight, and the compatilizer accounts for 8 parts by weight. Research shows that when the tungsten disulfide nanorod is 7.5-10 parts by weight and the compatilizer is 5-8 parts by weight, the obtained polypropylene composite material is more excellent in scratch resistance and mechanical property; when the tungsten disulfide nano rod accounts for 10 parts by weight and the compatilizer accounts for 8 parts by weight, the obtained polypropylene composite material has the best scratch resistance and mechanical property.
As a preferred embodiment of the polypropylene composite material of the present invention, the polypropylene composite material further comprises the following components in parts by weight: 1-10 parts of toughening agent and 1-10 parts of mineral filler.
As a preferred embodiment of the polypropylene composite material of the present invention, at least one of the following (a) to (e):
(a) the polypropylene is at least one of homo-polypropylene and co-polypropylene, the melt mass flow rate of the polypropylene is 0.3-100 g/10min, and the melt mass flow rate of the polypropylene is measured according to ISO 1133 by using 2.16kg weight and at 230 ℃;
(b) the average particle size of the tungsten disulfide nano-rods is 60-120 nm; the tungsten disulfide nanorod has too large particle size, stress concentration is easy to occur, and the product reinforcing effect is poor; the tungsten disulfide nano-rod has too small particle size and high inherent specific surface area, is easy to agglomerate and is difficult to disperse.
(c) The compatilizer is a polar monomer graft polymer, and the polymer in the polar monomer graft polymer is at least one of polyethylene, polypropylene, ethylene-alpha-ethylene-octene copolymer, styrene-butadiene copolymer, polyethylene-polystyrene-polypropylene copolymer, ethylene-propylene-butadiene copolymer, ethylene-acrylate copolymer and ethylene-acrylate-glycidyl methacrylate copolymer;
(d) the toughening agent is at least one of ethylene-octene copolymer and ethylene-butene copolymer, the toughening agent has the density of 0.8-0.9g/cm3 and the melt mass flow rate of 0.5-10 g/10min, and the melt mass flow rate of the toughening agent is measured according to ISO 1133 by using the weight of 2.16kg and at the temperature of 230 ℃;
(e) the mineral filler comprises inorganic powder with the particle size of 800-3000 meshes, and the inorganic powder is at least one of talcum powder, calcium carbonate, silicon dioxide and mica powder.
As a preferred embodiment of the polypropylene composite material, the tungsten disulfide nano-rods have an average particle size of 80 nm; the compatilizer is maleic anhydride grafted polypropylene.
As a preferred embodiment of the polypropylene composite material of the present invention, the polypropylene composite material further comprises the following components in parts by weight: 0.1-3.0 parts of processing aid and 0.5-3 parts of colorant.
As a preferred embodiment of the polypropylene composite material of the present invention, the processing aid comprises an antioxidant; the colorant is black master batch. The antioxidant can improve the antioxidant capacity of the polypropylene composite material and enhance the weather resistance of the polypropylene composite material.
As a preferred embodiment of the polypropylene composite material, the antioxidant is at least one of a phenol antioxidant, a phosphite antioxidant, a sulfur-containing antioxidant and an amine antioxidant; the black master batch is carbon black master batch, and the mass percentage of carbon black in the carbon black master batch is 30-45%.
The invention also provides a preparation method of the polypropylene composite material, which comprises the following steps:
(1) weighing the components according to the proportion;
(2) putting tungsten disulfide nanorods, a compatilizer, polypropylene accounting for 30-50% of the weight of all polypropylene and a processing aid accounting for 20-40% of the weight of all processing aids into an internal mixer for banburying, and then extruding and granulating by an extruder to obtain tungsten disulfide nanorod master batches;
(3) and (3) sequentially putting the rest polypropylene, the tungsten disulfide nanorod master batch obtained in the step (2), the toughening agent, the mineral filler, the colorant and the rest processing aid into a premixer, mixing uniformly, mixing, melting, homogenizing, and then extruding and granulating to obtain the polypropylene composite material.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the low-content tungsten disulfide nano-rods are introduced to improve the surface polarity of the polypropylene composite material and reduce the surface friction coefficient of the polypropylene composite material, so that the polypropylene composite material with surface scratch resistance and excellent mechanical properties is prepared. The polypropylene composite material meets the requirements of high performance and light weight of polypropylene materials.
In addition, the polypropylene composite material has simple preparation process and low production cost, and is suitable for large-scale mass production.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
In the examples described below, the melt Mass Flow Rates (MFR) of the polypropylene and the toughener are both measured according to ISO 1133 using a 2.16kg weight and at a temperature of 230 ℃.
Example 1
An example of the polypropylene composite material of the present invention is shown in Table 1.
The preparation method of the polypropylene composite material comprises the following steps:
(1) weighing the components according to the proportion;
(2) putting tungsten disulfide nanorods, a compatilizer, polypropylene accounting for 30-50% of the weight of all polypropylene and a processing aid accounting for 20-40% of the weight of all processing aids into an internal mixer for banburying, and then extruding and granulating by adopting a single screw extruder with an extrusion screw length-diameter ratio of 20:1 to obtain tungsten disulfide nanorod master batches;
(3) sequentially putting the rest polypropylene, the tungsten disulfide nanorod master batch obtained in the step (2), a toughening agent, a mineral filler, a coloring agent and the rest processing aid into a premixer, mixing uniformly, mixing, melting and homogenizing in an extruder with the length-diameter ratio of an extrusion screw being 48:1, and then extruding and granulating to obtain a polypropylene composite material; wherein the rotating speed of an extruder with the length-diameter ratio of an extrusion screw being 48:1 is 300-450r/min, and the temperature of each zone is as follows: the temperature of the T1 zone is 90-120 ℃, the temperature of the T2-T5 zone is 180-200 ℃, and the temperature of the T6-T12 zone is 200-220 ℃; the water length of the brace is 1-2M.
Examples 2 to 5
The components of the polypropylene composite materials described in the embodiments 2 to 5 are shown in table 1, and the preparation methods of the polypropylene composite materials described in the embodiments 2 to 5 are the same as those of the embodiment 1.
The polypropylene composite material of examples 1 to 5 was injection-molded into ISO mechanical sample strips and 200X 5X 2mm long plates by an injection molding machine, and then the tensile strength, bending strength, notch impact strength, abrasion and scratch resistance, surface Rockwell hardness, surface friction coefficient and other properties were measured. The test results are shown in table 1.
The method for testing each performance index comprises the following steps:
tensile strength test standard according to ISO 527-2, test conditions: the temperature is 23 ℃, and the stretching speed is 50 mm/min;
flexural strength test standard is according to ISO 178, test conditions: the temperature is 23 ℃, the bending rate is 2mm/min, and the span is 64 mm;
the notched impact strength test standard is in accordance with ISO 179-1eA, test conditions: the temperature is 23 ℃;
the abrasion and scratch resistance test standard is evaluated by a color difference value according to D421775, the color difference value test standard is PV 3952, and the test conditions are as follows: 10N.
The Rockwell hardness test standard of the surface is in accordance with GB/T3398.2, test conditions: the temperature is 23 ℃, and the thickness of the sample is 6 mm;
the surface friction coefficient test standard is according to ISO8295, test conditions: the temperature is 23 ℃, and the thickness of the sample piece is 0.5 mm.
TABLE 1
Example 6
In order to examine the influence of the content of the tungsten disulfide nanorods on the performance of the polypropylene composite material, the applicant prepares the polypropylene composite materials of a test group and a control group according to the method of the embodiment 1, and tests the performance of the polypropylene composite materials of the test group and the control group according to the method for testing the performance of the polypropylene composite materials of the embodiment 1-5.
In this example, the composition and properties of the polypropylene composites of the test and control groups are shown in table 2.
TABLE 2
In Table 2 above, the polypropylene was PP EP548R, a copolymer polypropylene having a melt flow rate of 28g/10min at a temperature of 230 ℃ and a load of 2.16kg, and purchased from Suzhou Guihai plastification Co., Ltd; the toughening agent is POE ENGAGE 7447, the melt flow rate is 1.2g/10min under the conditions of 230 ℃ and 2.16kg load, and the density is 0.862g/cm3Purchased from Suchang, Suzhou for plastication; the tungsten disulfide nano rod is 2000 meshes, has the grain diameter of 80nm and the crystal length of 0.3 mu m, and is purchased from Changshahua Jing powder material science and technology Limited company; mineral filler: talcum powder, TYT-777A, 3000 mesh, Xiamen Haichuan industrial and trade; the compatilizer is maleic anhydride grafted polypropylene, CMG9801, purchased from Jiangsu Co., Ltd, which is an easy compatilizer; the processing aid is a phenol antioxidant, an antioxidant 1010 and is purchased from wind, light and chemical industry limited company in Yingkou city; the colorant is black powder, black master batch with BB-576V and 40 percent of carbon black contentPurchased from maokang materials.
As shown in Table 2, when the tungsten disulfide nanorod accounts for 7.5-10 parts by weight, the obtained polypropylene composite material has more excellent scratch resistance and mechanical properties; when the weight of the tungsten disulfide nano rod is 10 parts, the obtained polypropylene composite material has the best scratch resistance and mechanical property.
Meanwhile, the applicant also investigated the influence of the content of the tungsten disulfide nanorods on the performance of the polypropylene composite material when the polypropylene, the toughening agent, the mineral filler, the compatilizer, the processing aid and the colorant are other substances and other parts by weight according to the above method, and all the results are consistent with those in table 2, which is not repeated herein.
Example 7
In order to examine the influence of the content of the compatilizer on the performance of the polypropylene composite material, the applicant prepares the polypropylene composite materials of a test group and a control group according to the method of the embodiment 1, and tests the performance of the polypropylene composite materials of the test group and the control group according to the method for testing the performance of the polypropylene composite materials described in the embodiments 1 to 5.
In this example, the composition and properties of the polypropylene composites of the test and control groups are shown in Table 3.
TABLE 3
In this example, the types and the manufacturers of polypropylene, toughener, tungsten disulfide nanoparticles, mineral filler, compatibilizer, processing aid, and colorant were the same as in example 6.
As shown in Table 3, in the invention, when the compatilizer is 5-8 parts by weight, the obtained polypropylene composite material has more excellent scratch resistance and mechanical property; when the compatilizer is 8 parts by weight, the obtained polypropylene composite material has the best scratch resistance and mechanical property.
Meanwhile, the applicant also investigated the influence of the content of the compatibilizer on the performance of the polypropylene composite material when the polypropylene, the toughening agent, the mineral filler, the tungsten disulfide nanorod, the processing aid and the colorant are other substances and other parts by weight according to the above method, and all the results are consistent with those in table 3, which is not repeated herein.
Example 8
In this example, the applicant investigated the influence of tungsten disulfide nanorods of different sizes on the performance of a polypropylene composite material, and in order to examine the influence, the applicant prepared polypropylene composite materials of different test groups according to the method of example 1, and tested the performance of the polypropylene composite materials of the test group and the control group according to the method for testing the performance of the polypropylene composite materials described in the above examples 1 to 5.
In this example, the composition and properties of the polypropylene composites of the test groups are shown in table 4.
TABLE 4
In this example, the types and the manufacturers of polypropylene, toughener, mineral filler, compatibilizer, processing aid and colorant were the same as in example 6; the tungsten disulfide nanorods are purchased from Changsha Huajing powder material science and technology limited, and the size is as follows:
tungsten disulfide nanorod-1: the mesh number is 2000 meshes, the grain diameter is 80nm, and the crystal length is 0.3 mu m;
tungsten disulfide nanorod-2: the mesh number is 800 meshes, the grain diameter is 80nm, and the crystal length is 0.3 mu m;
tungsten disulfide nanorod-2: the mesh number is 2000 meshes, the grain diameter is 200nm, and the crystal length is 0.3 mu m;
tungsten disulfide nanorod-2: 2000 mesh, particle size 80nm, crystal length 0.6 μm, Changsha Huajing powder materials science and technology Limited.
As can be seen from Table 4, when the number of the tungsten disulfide nanorods is 2000 meshes, the particle size is 80nm, and the crystal length is 0.3 μm, the obtained polypropylene composite material has the best scratch resistance and mechanical properties.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The polypropylene composite material is characterized by comprising the following components in parts by weight: 65-80 parts of polypropylene, 7.5-10 parts of tungsten disulfide nanorods, 5-8 parts of compatilizer, 1-10 parts of flexibilizer and 1-10 parts of mineral filler;
the compatilizer is a polar monomer graft polymer, and the polymer in the polar monomer graft polymer is at least one of polyethylene, polypropylene, ethylene-alpha-ethylene-octene copolymer, styrene-butadiene copolymer, polyethylene-polystyrene-polypropylene copolymer, ethylene-propylene-butadiene copolymer, ethylene-acrylate copolymer and ethylene-acrylate-glycidyl methacrylate copolymer; the toughening agent is at least one of ethylene-octene copolymer and ethylene-butene copolymer, and the density of the toughening agent is 0.8-0.9g/cm3The melt mass flow rate is 0.5-10 g/10min, and the melt mass flow rate of the toughening agent is measured at a temperature of 230 ℃ by using a weight of 2.16kg according to ISO 1133; the mineral filler comprises inorganic powder with the particle size of 800-3000 meshes, and the inorganic powder is at least one of talcum powder, calcium carbonate, silicon dioxide and mica powder.
2. The polypropylene composite according to claim 1, wherein the tungsten disulfide nanorods are 10 parts by weight and the compatibilizer is 8 parts by weight.
3. The polypropylene composite according to claim 1, wherein at least one of the following (a) to (b):
(a) the polypropylene is at least one of homo-polypropylene and co-polypropylene, the melt mass flow rate of the polypropylene is 0.3-100 g/10min, and the melt mass flow rate of the polypropylene is measured according to ISO 1133 by using 2.16kg weight and at the temperature of 230 ℃;
(b) the average particle size of the tungsten disulfide nano-rods is 60-120 nm.
4. The polypropylene composite of claim 3, wherein the tungsten disulfide nanorods have an average particle size of 80 nm; the compatilizer is maleic anhydride grafted polypropylene.
5. The polypropylene composite according to any one of claims 1 to 4, further comprising the following components in parts by weight: 0.1-3.0 parts of processing aid and 0.5-3 parts of colorant.
6. The polypropylene composite of claim 5, wherein the processing aid comprises an antioxidant; the colorant is black master batch.
7. The polypropylene composite according to claim 6, wherein the antioxidant is at least one of a phenolic antioxidant, a phosphite antioxidant, a sulfur-containing antioxidant, and an amine antioxidant; the black master batch is carbon black master batch, and the mass percentage of carbon black in the carbon black master batch is 30-45%.
8. A method for preparing a polypropylene composite material as claimed in any one of claims 5 to 7, comprising the steps of:
(1) weighing the components according to the proportion;
(2) putting tungsten disulfide nanorods, a compatilizer, polypropylene accounting for 30-50% of the weight of all polypropylene and a processing aid accounting for 20-40% of the weight of all processing aids into an internal mixer for banburying, and then extruding and granulating by an extruder to obtain tungsten disulfide nanorod master batches;
(3) and (3) sequentially putting the rest polypropylene, the tungsten disulfide nanorod master batch obtained in the step (2), the toughening agent, the mineral filler, the colorant and the rest processing aid into a premixer, mixing uniformly, mixing, melting, homogenizing, and then extruding and granulating to obtain the polypropylene composite material.
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| CN1990534A (en) * | 2005-12-28 | 2007-07-04 | 上海日之升新技术发展有限公司 | Process for preparing wear-resisting polypropene composite material for vehicle |
| CN106243510A (en) * | 2016-08-29 | 2016-12-21 | 合肥会通新材料有限公司 | A kind of high abrasion modified polypropylene composite material and preparation method thereof |
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| KR101402502B1 (en) * | 2008-12-22 | 2014-06-19 | 바스프 에스이 | Method of improving scratch resistance and related products and uses |
| ES2361449B1 (en) * | 2009-12-04 | 2012-04-20 | CONSEJO SUPERIOR DE INVESTIGACIONES CIENT�?FICAS (CSIC) (Titular al 50%) | NANOCOMPUESTOPS MATERIALS OF POLYPROPYLENE AND CARBON NITRURES, PROCEDURES FOR THEIR OBTAINING AND APPLICATIONS. |
| CN102586927B (en) * | 2012-03-01 | 2013-11-27 | 中国人民解放军总后勤部军需装备研究所 | Ultrahigh molecular weight polyethylene/nano tungsten disulfide composite fiber and preparation method and application thereof |
| KR101617176B1 (en) * | 2014-08-27 | 2016-05-18 | 경희대학교 산학협력단 | Organic-inorganic nano composite and method for manufaturing the same |
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| CN1990534A (en) * | 2005-12-28 | 2007-07-04 | 上海日之升新技术发展有限公司 | Process for preparing wear-resisting polypropene composite material for vehicle |
| CN106243510A (en) * | 2016-08-29 | 2016-12-21 | 合肥会通新材料有限公司 | A kind of high abrasion modified polypropylene composite material and preparation method thereof |
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