CN113527812A - Low-odor interior trim composite polypropylene for vehicle and preparation method thereof - Google Patents
Low-odor interior trim composite polypropylene for vehicle and preparation method thereof Download PDFInfo
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to the technical field of automotive interior materials, and discloses a low-odor automotive interior composite polypropylene and a preparation method thereof, wherein flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder and niobate are used as lubricating additives and are compounded with high-melt index polypropylene, and a pretreatment material is obtained through blending, extrusion and granulation; and then adding the polypropylene, the filler and the pretreatment material into a high-speed mixer, uniformly mixing, adding a feed inlet of a parallel double-screw extruder, extruding through a perforated plate die head, carrying out water cooling, air drying, cutting into granules by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene. The composite polypropylene material obtained by the formula and the process has excellent smoothness, scratch resistance and black and bright color, is very suitable for processing automotive upholsteries and instrument panels, reduces the volatile odor of polypropylene, and can reduce the subsequent injection molding processing temperature to prevent the degradation of the polypropylene.
Description
Technical Field
The invention relates to the technical field of automotive interior materials, in particular to low-odor automotive interior composite polypropylene and a preparation method thereof.
Background
Polypropylene is used as plastic with easy processing, good heat resistance, good stability and high strength, and the application proportion of the polypropylene in automobile interior decoration is higher and higher. However, with the improvement of the use ratio of polypropylene in the automotive interior, the volatile smell of polypropylene has more and more obvious influence on the quality of air in the automobile, and the smell in the automobile directly influences the quality of the automobile and influences the human health and the ecological environment. In order to ensure the safety in the automobile, the evaluation guideline of the air quality in the passenger car becomes a mandatory standard, and strict requirements are made on the air quality in the automobile. The polypropylene for automobile interior is used in a large amount and in a large variety, and therefore, it is important to develop low-odor polypropylene suitable for automobile interior.
According to the current research conclusion, the volatile odor of polypropylene mainly comes from two aspects, one is that: in the process of preparing polypropylene by polymerization, a catalyst and a chemical solvent are needed, and a monomer is easy to remain and becomes a volatile main component, and at present, better progress is made mainly by improving the polymerization process and method of polypropylene, such as reducing the monomer residue by adopting a hydrogenation method for polymerization and the like; another aspect is: polypropylene needs to be processed into various shapes of interior parts in the processes of compounding, injection molding and the like, and the polypropylene is required to have good smooth flowability, wear resistance, smoothness, flame retardance and the like, so that various functional additives such as polyethylene wax, polypropylene wax and the like are added into the polypropylene during processing to improve the dispersibility of pigments, and erucamide is added to improve the smoothness of products, but the additives with relatively low molecular weight are easy to degrade during heating, so that odorous substances are generated.
In order to solve the odor generated by the processing aid, at present, a porous material with an adsorption function is mainly added into polypropylene, and adsorption materials such as activated carbon, silica gel, metal oxide, attapulgite, molecular sieves and the like are generated. When the adsorption systems are distributed in a resin matrix in a certain form, the adsorption systems can adsorb odor or volatile small molecules generated by the resin. However, the effect of the porous material for adsorbing the volatile matter of the volatile auxiliary is limited, and the porous material with too much porous adsorbent has a high oil absorption value, so that the lubricating auxiliary is adsorbed, thereby reducing the lubricating and smooth effect.
Chinese invention patent publication No. CN109721832A discloses a low-odor polypropylene composition for automobiles and a preparation method thereof, which is prepared from 80-100 parts of polypropylene, 20-30 parts of a toughening agent, 1-2 parts of an antioxidant, 0.5-1 part of a lubricant and 10-15 parts of odor adsorption master batches; the odor adsorption master batch uses the magnesium sulfate whisker and the bamboo charcoal powder, has high oil absorption value although having adsorption to odor, and adsorbs a lubricant while adsorbing the odor, so that the lubricating effect is reduced.
In order to reduce the volatile odor of polypropylene and prevent the porous physical adsorbent from reducing the processing lubricity of plastics, it is necessary to provide a novel composite polypropylene material, and further to obtain a polypropylene automotive interior material with low odor suitable for processing.
Disclosure of Invention
Aiming at solving the problem that the machining lubricity of plastics is affected by a porous physical adsorbent used for solving the odor of polypropylene volatile matters, the invention provides the low-odor automotive interior composite polypropylene and a preparation method thereof, so that the odor of the polypropylene volatile matters is reduced, and the porous physical adsorbent is prevented from reducing the machining lubricity of the plastics.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-odor automotive interior trim composite polypropylene is prepared by blending, extruding and granulating polypropylene, a filler and a pretreatment material.
Preferably, the filler is carbon black.
Preferably, the pretreatment material is obtained by blending, extruding and granulating flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder, niobate and high-melt index polypropylene.
Preferably, in the composite polypropylene, the mass ratio of the polypropylene to the filler to the pretreatment material is 100: 10: 15-20.
Preferably, in the pretreatment material, the mass ratio of flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder, niobate and high-melt index polypropylene is 15-20: 0.5-1: 5-10: 3-5: 1-2: 30-50.
Preferably, the flake graphite is natural flake graphite.
Further preferably, the carbon content of the natural crystalline flake graphite is not less than 94%, and the particle size is not more than 38 μm.
Preferably, the content of barium sulfate in the nano spherical barium sulfate is not less than 99%, the particle size is not more than 0.3 μm, and the sphericity is not less than 90%.
Preferably, the particle size of the nano serpentine powder is not higher than 0.3 μm.
Preferably, the niobate is LiNbO3、 K4Nb6O17、KNb3O8One of (1);
preferably, the high melt index polypropylene has a melt index greater than 30g/10 min.
Further preferably, the high-fluidity polypropylene is S2040 polypropylene.
The invention also provides a preparation method of the low-odor interior trim composite polypropylene for the vehicle, which is characterized by comprising the following steps of:
(1) adding flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder, niobate and high-melt index polypropylene into a high-speed mixer, uniformly mixing, and then carrying out melt extrusion granulation by a screw extruder to obtain a pretreatment material;
(2) adding polypropylene, filler and pretreatment materials into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a perforated plate die head, and carrying out water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene.
Preferably, the heating temperature of each section of the extruder in the step (1) is as follows: one section is 155-165 ℃, the second section is 170-180 ℃, the third section is 170-180 ℃, and the fourth section is 150-160 ℃.
Preferably, the screw of the extruder in step (1) is provided with a secondary vacuum, and volatile components are exhausted in vacuum.
Preferably, the heating temperature of each section of the extruder in the step (2) is as follows: the temperature of one section is 160 ℃ to 180 ℃, the temperature of the second section is 180 ℃ to 190 ℃, the temperature of the third section is 180 ℃ to 190 ℃, and the temperature of the fourth section is 160 ℃ to 170 ℃.
The known crystalline flake graphite is natural crystalline graphite which is similar to fish phosphorus in shape, belongs to a hexagonal crystal system, has a layered structure, is complete in crystallization, thin in sheet, good in toughness and excellent in physical and chemical properties, has good high temperature resistance, electric conduction, heat conduction, lubrication, plasticity, acid and alkali resistance and the like, and is a natural solid lubricant with the layered structure; graphene is a new material formed by tightly stacking sp hybridized and connected carbon atoms into a single-layer two-dimensional honeycomb lattice structure, is difficult to exist in a single-layer form, usually exists in a multi-layer graphene structure, has chemical properties similar to those of graphite, can adsorb and desorb various atoms and molecules, and has a lubricating effect; barium sulfate has the advantages of strong chemical inertia, good stability, acid and alkali resistance, moderate hardness, high specific gravity, high whiteness, capability of absorbing harmful rays and the like, has high thermal conductivity and high rheological property, and is a good lubricating dispersant; the nano serpentine is a hydrous magnesium silicate with a layered structure, has an extremely low friction coefficient, does not react with resin or change the properties of the resin, and is an ideal lubricating additive; niobate is also a layered substance having good lubricity and has unique electromagnetic properties and redox activity.
In the prior art, a micromolecular lubricant is usually added into polypropylene to improve the processing performance, and a porous adsorbent is further added for adsorption in order to solve the problem of the odor of the auxiliary agent. However, it is known that the porous adsorbent has a limited adsorption amount and poor selective adsorption performance, and cannot realize long-term adsorption, and the porous adsorbent has a high oil absorption value, so that the lubricant is adsorbed, thereby reducing the lubricating and slipping effects. According to the method, an organic lubricating additive is not added into polypropylene, but flake graphite with excellent sliding property, graphene, nano spherical barium sulfate, nano serpentine powder and niobate are compounded to serve as a lubricating additive, so that the problem of odor caused by migration, escape, volatilization and the like of a small molecular lubricant is solved.
Further, high-melt-index polypropylene is adopted to carry out dispersion treatment on flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder and niobate, the high-melt-index polypropylene can realize good surface coating on the flake graphite, the nano spherical barium sulfate, the nano serpentine powder and the niobate, and can be filled between the flakes of the flake graphite, the niobate and the nano serpentine to endow the flake graphite, the nano spherical barium sulfate, the nano serpentine powder and the niobate with excellent processing flowability, and the high-melt-index polypropylene, the nano spherical barium sulfate, the nano serpentine powder and the niobate are cooperatively used for the polypropylene, so that the processing flowability of materials is greatly increased, and the subsequent injection molding processing temperature is reduced. The method of the invention not only reduces the odor of volatile matters of the polypropylene and improves the processing performance, but also can prevent the polypropylene from being degraded due to overhigh injection processing temperature.
Furthermore, the niobate has good lubricity, unique electromagnetic property and redox activity, and can decompose residual organic pollutants under the condition of proper wavelength, thereby further reducing the odor of the polypropylene material. The nano spherical barium sulfate with high sphericity can move in a rolling mode in the system, so that the moving friction force is reduced, and the processing fluidity is favorably improved.
The existing micromolecule lubricant is easy to migrate, escape and volatilize from a matrix, volatile smell is caused, the polypropylene material is difficult to meet the air quality standard in the vehicle, the adsorption capacity of the porous adsorbent is limited, the selective adsorption performance is poor, and long-term adsorption cannot be realized. In view of the above, the invention provides a low-odor automotive interior composite polypropylene and a preparation method thereof, which comprises the steps of compounding flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder and niobate serving as lubricating additives with high-melt index polypropylene, and obtaining a pretreatment material through blending, extrusion and granulation; and then adding the polypropylene, the filler and the pretreatment material into a high-speed mixer, uniformly mixing, adding a feed inlet of a parallel double-screw extruder, extruding through a perforated plate die head, carrying out water cooling, air drying, cutting into granules by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene. The composite polypropylene material obtained by the formula and the process has excellent smoothness, scratch resistance and black and bright color, and is very suitable for processing automotive upholsteries and instrument panels.
The invention provides low-odor automotive interior composite polypropylene and a preparation method thereof, and compared with the prior art, the low-odor automotive interior composite polypropylene has the outstanding characteristics and excellent effects that:
1. according to the invention, the flake graphite, the graphene, the nano spherical barium sulfate, the nano serpentine powder and the niobate with excellent sliding property are compounded to be used as the lubricating additive, so that the odor problems caused by migration, escape, volatilization and the like of the small molecular lubricant are solved.
2. The high-melt-index polypropylene is adopted to carry out dispersion treatment on the flake graphite, the nano spherical barium sulfate, the nano serpentine powder and the niobate, so that the flake graphite, the nano spherical barium sulfate, the nano serpentine powder and the niobate are endowed with excellent processing flowability and are cooperatively used for the polypropylene, the processing flowability of materials is greatly increased, the subsequent injection molding processing temperature is reduced, and the polypropylene degradation caused by overhigh injection molding processing temperature is prevented.
3. The niobate used by the invention not only has good lubricity, but also has unique electromagnetic property and redox activity, and can decompose residual organic pollutants under the condition of proper wavelength, thereby further reducing the odor of the polypropylene material.
4. The composite polypropylene material prepared by the invention has excellent smoothness, scratch resistance and black and bright color, and is very suitable for processing automotive upholsteries and instrument panels.
Drawings
FIG. 1: example 1 sample of material injection molded; the surface of the sample is uniform and smooth.
FIG. 2: the sample injection molded from the material of comparative example 5 had poor flowability and poor surface uniformity.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And Shanghai Siceco polypropylene S2040 in a mass ratio of 15: 0.5: 10: 5: 1: 50, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 20, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Example 2
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And Shanghai Siceco polypropylene S2040 in a mass ratio of 15: 0.6: 5: 5: 2: 40, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: one section is 155 ℃, the second section is 170 ℃, the third section is 180 ℃, and the fourth section is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 18, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one at 160 deg.C, two at 180 deg.C, three at 180 deg.C, and four at 160 deg.C.
Example 3
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And the Shanghai Siceco polypropylene S2040 is prepared by mixing the following components in a mass ratio of 20: 0.8: 10: 3: 1: 40, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 175 ℃, the third stage is 175 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 18, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 170 deg.C, two 185 deg.C, three 185 deg.C and four 165 deg.C.
Example 4
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And the Shanghai Siceco polypropylene S2040 is prepared by mixing the following components in a mass ratio of 20: 1: 5: 5: 2: 30, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 15, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Example 5
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And the Shanghai Siceco polypropylene S2040 is prepared from the following components in a mass ratio of 15: 0.5: 8: 4: 1.5: 40, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: one section is 160 ℃, the second section is 175 ℃, the third section is 175 ℃, and the fourth section is 155 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 18, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 170 deg.C, two 185 deg.C, three 185 deg.C and four 165 deg.C.
Comparative example 1
(1) Flake crystalline flake graphite with the granularity of less than 38 mu m, graphene nanosheet, nano spherical barium sulfate with the grain diameter of less than 0.3 mu m and the sphericity of more than 90 percent, and niobate KNb3O8And Shanghai Siceco polypropylene S2040 in a mass ratio of 15: 0.5: 10: 1: 50, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 20, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 1 compared to example 1, no nano serpentine was added to the pretreatment, and the rest was identical to example 1.
Comparative example 2
(1) Preparing graphene nano-sheets, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90 percent, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And Shanghai Siceco polypropylene S2040 in a mass ratio of 0.5: 10: 5: 1: 50, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 20, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 2 in comparison to example 1, no flake graphite was added to the pretreatment, and the rest was identical to example 1.
Comparative example 3
(1) Flake crystalline flake graphite with the particle size of less than 38 mu m, graphene nanosheet, nano serpentine powder with the particle size of less than 0.3 mu m and niobate KNb3O8And Shanghai Siceco polypropylene S2040 in a mass ratio of 15: 0.5: 5: 1: 50, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein each section of the extruderThe heating temperature of (a) is: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 20, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 3 compared to example 1, the pretreatment material was completely identical to example 1 except that the nano-spherical barium sulfate was not added.
Comparative example 4
(1) Flake crystalline flake graphite with the granularity of less than 38 mu m, graphene nanosheets, nano spherical barium sulfate with the particle size of less than 0.3 mu m and the sphericity of more than 90%, nano serpentine powder with the particle size of less than 0.3 mu m and polypropylene S2040 of Shanghai Seisaceae in a mass ratio of 15: 0.5: 10: 5: 50, adding the mixture into a high-speed mixer, uniformly mixing, then carrying out melt extrusion granulation by a screw extruder, and setting secondary vacuum on a screw to obtain a pretreated material; wherein the heating temperature of each section of the extruder is as follows: the first stage is 165 ℃, the second stage is 180 ℃, the third stage is 180 ℃, and the fourth stage is 160 ℃;
(2) mixing Yanshan petrochemical K1712 polypropylene, carbon black and a pretreatment material according to a mass ratio of 100: 10: 20, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 4 in comparison to example 1, no niobate was added to the pretreatment batch, and the rest was identical to example 1.
Comparative example 5
Mixing Yanshan petrochemical K1712 polypropylene and carbon black according to the mass ratio of 100: 10, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 5 compared to example 1, no pretreatment was added, and the rest was identical to example 1.
Comparative example 6
According to the mass ratio of 100: 10: 4, adding the mixture into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a porous plate die head, and performing water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the automotive interior composite polypropylene; wherein the heating temperature of each section of the extruder is as follows: one 180 deg.c, two 190 deg.c, three 190 deg.c and four 170 deg.c.
Comparative example 6 compared to example 1, a polyethylene wax was used as a lubricant additive, the others being identical to example 1.
The test method comprises the following steps:
and (3) testing the melting property: according to the method for measuring the melt flow index of GB/T3682, the melt index of the composite polypropylene is measured under the conditions of 230 ℃ and 2.16kg, and the test results are shown in Table 1;
processing fluidity test: weighing 400g of the materials in the example 1 and the comparative example 5 respectively, and hot-pressing at 180 ℃ to form sample wafers, wherein the attached figure 1 shows that the sample wafers hot-pressed by the materials in the example 1 have good fluidity and uniform and smooth surfaces; FIG. 2 is a sample wafer of comparative example 5, which has poor material flowability at 180 ℃ and poor surface uniformity;
and (3) testing the odor performance: weighing 400g of the materials in the examples 1-5 and the materials in the comparative examples 1-6, performing injection molding on a sample at 180 ℃ to obtain a plate with the thickness of 3mm and the side length of 15cm, naturally cooling to room temperature, sending the plate into a closed chamber at 80 ℃ for treatment for 2h, reducing the temperature to 60 ℃, and judging the volatile odor grade in the closed chamber; then, processing for 4 hours at the wavelength of 320-350nm of an ultraviolet lamp and the power of 100W/cm, sending the plate into a closed chamber at the temperature of 80 ℃ for processing for 2 hours, reducing the temperature to 60 ℃, and judging the grade of the volatile smell in the closed chamber; the characterization method comprises the following steps: level 1: no smell; and 2, stage: smelling, without interfering smell; and 3, level: obvious smell without interference; 4, level: strong smell is generated; the test results are shown in table 2.
Table 1:
| performance index | Melt flow index (g/10 min) | Performance index | Melt flow index (g/10 min) |
| Example 1 | 36.7 | Comparative example 1 | 25.8 |
| Example 2 | 35.2 | Comparative example 2 | 28.3 |
| Example 3 | 36.8 | Comparative example 3 | 22.6 |
| Example 4 | 36.2 | Comparative example 4 | 29.1 |
| Example 5 | 35.9 | Comparative example 5 | 14.2 |
| Comparative example 6 | 17.1 |
Table 2:
| performance index | Primary odor grade | Odor rating after light treatment |
| Example 1 | Grade 3 | Stage 2 |
| Example 2 | Grade 3 | Stage 2 |
| Example 3 | Grade 3 | Stage 2 |
| Example 4 | Grade 3 | Stage 2 |
| Example 5 | Grade 3 | Stage 2 |
| Comparative example 1 | Grade 3 | Stage 2 |
| Comparative example 2 | Grade 3 | Stage 2 |
| Comparative example 3 | Grade 3 | Stage 2 |
| Comparative example 4 | Grade 3 | Grade 3 |
| Comparative example 5 | Grade 3 | Grade 3 |
| Comparative example 6 | 4 stage | Grade 3 |
Claims (8)
1. The low-odor automotive interior composite polypropylene is obtained by blending, extruding and granulating polypropylene, filler and pretreatment materials, and is characterized in that: the filler is carbon black; the pretreatment material is prepared by blending, extruding and granulating flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder, niobate and high-melt index polypropylene.
2. The low-odor composite polypropylene for automotive interior trim of claim 1, wherein the mass ratio of the polypropylene to the filler to the pretreatment material is 100: 10: 15-20.
3. The low-odor automotive interior composite polypropylene of claim 1, wherein the mass ratio of the flake graphite, the graphene, the nano spherical barium sulfate, the nano serpentine powder, the niobate and the high-melt index polypropylene in the pretreatment material is 15-20: 0.5-1: 5-10: 3-5: 1-2: 30-50.
4. The low odor automotive interior composite polypropylene of claim 1, wherein:
the flake graphite is natural flake graphite; the carbon content of the natural crystalline flake graphite is not lower than 94%, and the particle size is not higher than 38 mu m;
the content of barium sulfate in the nano spherical barium sulfate is not less than 99%, the particle size is not more than 0.3 mu m, and the sphericity is not less than 90%;
the particle size of the nano serpentine powder is not higher than 0.3 mu m;
the niobate is LiNbO3、 K4Nb6O17、KNb3O8One of (1);
the melt index of the high-melt index polypropylene is more than 30g/10 min.
5. The preparation method of the low-odor composite polypropylene for automotive interiors, as claimed in any of claims 1 to 4, is characterized by comprising the following steps:
(1) adding flake graphite, graphene, nano spherical barium sulfate, nano serpentine powder, niobate and high-melt index polypropylene into a high-speed mixer, uniformly mixing, and then carrying out melt extrusion granulation by a screw extruder to obtain a pretreatment material;
(2) adding polypropylene, filler and pretreatment materials into a high-speed mixer, uniformly mixing, adding the mixture into a feed inlet of a parallel double-screw extruder, extruding the mixture through a perforated plate die head, and carrying out water cooling, air drying, particle cutting by a hob and packaging on extruded strips to obtain the low-odor automotive interior composite polypropylene.
6. The method for preparing the low-odor composite polypropylene for automotive interior trim according to claim 5, wherein the heating temperature of each section of the extruder in the step (1) is as follows: one section is 155-165 ℃, the second section is 170-180 ℃, the third section is 170-180 ℃, and the fourth section is 150-160 ℃.
7. The method for preparing the low-odor composite polypropylene for automotive interiors according to claim 5, wherein in the step (1), the screw of the extruder is provided with secondary vacuum, and volatile components are evacuated.
8. The method for preparing the low-odor composite polypropylene for automotive interior trim according to claim 5, wherein the heating temperature of each section of the extruder in the step (2) is as follows: the temperature of one section is 160 ℃ to 180 ℃, the temperature of the second section is 180 ℃ to 190 ℃, the temperature of the third section is 180 ℃ to 190 ℃, and the temperature of the fourth section is 160 ℃ to 170 ℃.
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| CN114085529A (en) * | 2021-12-28 | 2022-02-25 | 中国科学院兰州化学物理研究所 | Polyphenylene sulfide-based self-lubricating multi-element composite material and preparation method thereof |
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| CN114085529A (en) * | 2021-12-28 | 2022-02-25 | 中国科学院兰州化学物理研究所 | Polyphenylene sulfide-based self-lubricating multi-element composite material and preparation method thereof |
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