CN111500008A - Flame-treatment-free polypropylene material and preparation method and application thereof - Google Patents
Flame-treatment-free polypropylene material and preparation method and application thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- 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
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a flame-free polypropylene material and a preparation method and application thereof, which are prepared from 60-85 parts of polypropylene, 0-25 parts of inorganic filler, 4-12 parts of toughening agent, 2-6 parts of polar auxiliary agent, 0.2-1 part of antioxidant and 0.2-1 part of other auxiliary agent according to parts by weight, wherein the polar auxiliary agent is a composite of polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene. The polypropylene material has high surface tension, can be subjected to slush molding and foaming without flame treatment, and can keep excellent mechanical properties while improving the adhesive force with a polyurethane foaming layer.
Description
Technical Field
The invention belongs to the field of modification of high polymer materials, and particularly relates to a flame-free polypropylene material, and a preparation method and application thereof.
Background
With the development of the automobile industry and the gradual improvement of the living demands of people, the competition among various automobile manufacturers is more and more intense, the cost, the environmental protection, the energy conservation and the emission reduction of automobile materials are more and more increased, and polypropylene becomes a mainstream material of automobile interior and exterior decorations due to the extremely low density, the non-toxicity, the environmental protection, the low price and the excellent comprehensive performance of the polypropylene, gradually replaces plastics such as PVC, ABS, PC and the like, and becomes the most widely applied plastic material on automobile ornaments.
Because of the aesthetic requirements of appearance, automotive interior parts such as instrument panels, columns and the like are generally improved in visual sense and good touch sense by adopting a slush molding foaming process, polypropylene belongs to a nonpolar material, and polyurethane of a slush molding foaming layer is a polar material and is incompatible with the polypropylene. At present, the flame treatment method is mainly adopted to improve the polarity of the surface of the polypropylene part and enhance the cohesiveness of the polypropylene part and the polypropylene part, but the flame treatment process has higher cost and complex working procedures. To improve efficiency and reduce cost, it is necessary to develop a polypropylene material that does not require flame treatment.
In the prior art, a polypropylene composite for a flame-free instrument panel is prepared by combining a non-polar elastomer and a polar elastomer to increase the surface tension to a level sufficient for slush molding foaming, wherein the polar elastomer is one or a mixture of two or more of ethylene/vinyl acetate copolymer, ethylene/acrylate/maleic anhydride and ethylene/acrylate/glycidyl methacrylate copolymer. In addition, the polypropylene composite without flame treatment and the preparation method thereof are provided, and the polarity of polypropylene can be improved by adding ethylene-vinyl acetate copolymer into the polypropylene material, so that the aim of directly spraying without flame treatment can be achieved. The prior art also discloses a flame-free sprayable polypropylene composite material and a preparation method thereof, wherein the flame-free sprayable polypropylene composite material can be sprayed without flame treatment and has good paint adhesion by the synergistic effect of 0-3% of compatilizer and 0-1% of surface lubricant. However, the above technical solutions all have the problem that the compatibility and mechanical properties of the polar matrix and polypropylene are reduced.
Disclosure of Invention
In view of the above, the invention needs to provide a flame-free polypropylene material, and a preparation method and an application thereof, wherein a polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene composite is added into a system, so as to improve the surface tension of the polypropylene material, enable slush molding and foaming without flame treatment, improve the adhesion with a polyurethane foaming layer, maintain excellent mechanical properties, and solve the problems of the prior art that the compatibility and mechanical properties of a polar matrix and polypropylene are reduced.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a flame-free polypropylene material, which is prepared from 60-85 parts of polypropylene, 0-25 parts of inorganic filler, 4-12 parts of toughening agent, 2-6 parts of polar auxiliary agent, 0.2-1 part of antioxidant and 0.2-1 part of other auxiliary agent in parts by weight, wherein the polar auxiliary agent is a composite of polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene.
Further, the polypropylene is at least one of block copolymerization polypropylene and homopolymerization polypropylene, and the melt flow rate of the polypropylene under the test condition of 230 ℃/2.16KG is 1-100g/10 min.
Further, the inorganic filler is at least one of talcum powder, calcium carbonate, wollastonite, mica and barium sulfate, and the particle size of the inorganic filler is 1-10 mu m.
Further, the toughening agent is at least one of ethylene-butylene copolymer and ethylene-octene copolymer, and the density of the toughening agent is 0.88-0.90g/cm3The melt index at 190 ℃/2.16KG is between 0.5 and 30g/10 min.
The primary antioxidant and the secondary antioxidant may be selected conventionally in the art, the hindered phenolic antioxidant may be selected from at least one of 1010, 1076 and 3114, the thioester antioxidant may be selected from at least one of DSTP, D L TP and DMTP, and the phosphite antioxidant may be selected from at least one of 168, 618 and 626, it being understood that specific examples of the antioxidant in the present invention include, but are not limited to, the above.
Further, the other auxiliary agents comprise at least one of low molecular weight esters, metal soaps and stearic acid complex esters. Comprises PE wax, EBS, stearic acid, calcium stearate and zinc stearate, and is mainly used for lubricating and dispersing. It is understood that other additives may be selected, and the addition of the corresponding additives is within the scope of the art according to the desired properties, etc., and will not be described in detail herein.
Further, the polypropylene-maleic acid alternating copolymer has a number average molecular weight of 1000-2500, an acid value of 30-60, and a structural formula:
according to the structural formula, a plurality of adjacent maleic acid compounds are arranged in each molecule, the maleic anhydride groups have higher polarity, and a plurality of maleic anhydride groups and the polar acrylic groups of the acrylic grafted polypropylene react with isocyanate in the polyurethane component to form chemical bonds. Thereby greatly increasing the adhesive force of the polypropylene material and the polyurethane foaming layer.
Further, in the polar auxiliary agent, the polypropylene-maleic acid alternating copolymer and the acrylic acid grafted polypropylene are mixed, wherein the weight ratio of the polypropylene-maleic acid alternating copolymer in the polar auxiliary agent is 20-80%.
The second aspect of the present invention provides a method for preparing a flame-free polypropylene material according to the first aspect of the present invention, comprising the following steps:
fully mixing polypropylene, inorganic filler, toughening agent, polar additive, antioxidant and other additives according to a ratio to obtain a uniform mixed material;
and adding the mixed material into a double-screw extruder, and carrying out melting, extrusion, grain cutting and drying to obtain granules. Wherein the temperature of a material cylinder of the double-screw extruder is 190-230 ℃, the rotating speed of a screw is 400-450r/min, the rotating speed of a main machine is 18-20Hz, and the vacuum degree is-0.07-0.08 MPa.
The third aspect of the present invention provides the use of the flame-free treated polypropylene material according to the first aspect of the present invention for the preparation of automotive interior trim parts.
Compared with the prior art, the polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene compound is added into a polypropylene system, and the high-polarity maleic anhydride group of the polypropylene-maleic acid alternating copolymer and the polar acrylic group of the acrylic acid grafted polypropylene react with isocyanate in the polyurethane component to form a chemical bond, so that the surface tension of the product is improved to a level sufficient for slush molding foaming, and slush molding foaming can be carried out without adding a flame treatment process. Compared with maleic anhydride grafted polypropylene, each molecule of the polypropylene-maleic acid alternating copolymer has a plurality of adjacent maleic acid compounds, the adhesive force with the polyurethane foaming layer is greatly increased, and the flame-free polypropylene material also has excellent mechanical properties. Therefore, compared with the prior art, the material provided by the invention greatly reduces the production cost of slush molding foaming products.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
In the composite formulations of the examples and comparative examples:
the polypropylene is block copolymerized propylene with melt flow rate (230 deg.C × 2.16.16 kg) of 5-60/10min, wherein the comonomer of the block copolymerized propylene is ethylene, the content of which is in the range of 4-10 mol%, and the mark is EP548 RQ;
the inorganic filler is talcum powder with the average diameter of 5 mu m;
the toughening agent is ethylene-butylene copolymer L C565 of L G company;
the polar assistant is polypropylene-maleic acid alternating copolymer (Baker hughes X-10016) and acrylic acid grafted PP, and the mark (BYK TPPP 5411 FA);
the antioxidant is Irganox 1010 (chemical name is tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester) from Ciba and Igrafos168 (chemical name is tris (2, 4-di-tert-butylphenyl) phosphite) from Ciba.
The processing aid was Cast (calcium stearate) from hair base italy.
Example 1
Weighing 83.4 parts of polypropylene, 10 parts of talcum powder, 4 parts of toughening agent, 2 parts of polypropylene-maleic acid alternating copolymer, 1 part of acrylic acid grafted PP, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 2
Weighing 83.4 parts of polypropylene, 10 parts of talcum powder, 4 parts of toughening agent, 0.5 part of polypropylene-maleic acid alternating copolymer, 2 parts of acrylic acid grafted PP, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 3
Weighing 81.4 parts of polypropylene, 10 parts of talcum powder, 4 parts of toughening agent, 3 parts of polypropylene-maleic acid alternating copolymer, 3 parts of acrylic acid grafted PP, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 4
Weighing 65.4 parts of polypropylene, 20 parts of talcum powder, 10 parts of toughening agent, 4 parts of polypropylene-maleic acid alternating copolymer, 1 part of acrylic acid grafted PP, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 5
Weighing 63.4 parts of polypropylene, 20 parts of talcum powder, 10 parts of toughening agent, 4 parts of polypropylene-maleic acid alternating copolymer, 2 parts of acrylic acid grafted PP, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 6
Weighing 60 parts of polypropylene, 4 parts of a toughening agent, 1 part of a polypropylene-maleic acid alternating copolymer, 1 part of acrylic acid grafted polypropylene, Irganox 10100.1 parts, Igrafos 1680.1 parts and 0.2 part of Cast according to parts by weight, dry-mixing in a high-speed mixer for 5 minutes, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Example 7
Weighing 85 parts of polypropylene, 25 parts of talcum powder, 12 parts of toughening agent, 4 parts of polypropylene-maleic acid alternating copolymer, 2 parts of acrylic acid grafted polypropylene, Irganox 10100.5 parts, Igrafos 1680.5 part and Cast 1 part in parts by weight, dry-mixing for 5 minutes in a high-speed mixer, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Comparative example 1
Weighing 85.4 parts of polypropylene, 10 parts of talcum powder, 4 parts of toughening agent, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing for 5 minutes in a high-speed mixer, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Comparative example 2
Weighing 69.4 parts of polypropylene, 20 parts of talcum powder, 10 parts of toughening agent, 0.2 part of Irganox 1010, 0.2 part of Igrafos168 and 0.2 part of Cast in parts by weight, dry-mixing for 5 minutes in a high-speed mixer, adding into a double-screw extruder, and carrying out melt extrusion granulation, wherein the temperature in a screw cylinder is as follows: the first zone is 200 ℃, the second zone is 210 ℃, the third zone is 210 ℃, the fourth zone is 210 ℃, the head is 220 ℃, and the rotating speed of the double-screw extruder is 400 r/min. Drying the particles, and performing injection molding on an injection molding machine to prepare a sample.
Test example
The sample density test is carried out according to the ISO1183-1 standard, the bending performance test is carried out according to the ISO178 standard, the sample size is 80 × 10 × 4mm, the span is 64mm, the bending speed is 2mm/min, the impact performance test of the simply supported beam is carried out according to the ISO179-1 standard, the sample size is 80 × 10 × 4mm, the notch depth is one third of the thickness of the sample, the melt flow rate is carried out according to the ISO1133-1 standard, the test condition is 230 ℃ × 2.16.16 kg, the surface tension is tested by directly connecting a dyne on a sample plate, the sample plate is directly foamed by polyurethane without flame treatment and then is subjected to the peel force test, and the test structure is shown in the following table 1:
TABLE 1 results of Performance test in examples 1 to 5 and comparative examples 1 to 2
Through comparison between comparative examples 1-2 and examples 1-5, we can find that the flame-free polypropylene material of the invention significantly improves the surface tension value of the polypropylene material compared with the prior art, and meets the requirement of flame-free treatment, and simultaneously the mechanical property of the flame-free polypropylene material still keeps excellent and can meet the use requirement.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The flame-free polypropylene material is characterized by being prepared from 60-85 parts of polypropylene, 0-25 parts of inorganic filler, 4-12 parts of toughening agent, 2-6 parts of polar auxiliary agent, 0.2-1 part of antioxidant and 0.2-1 part of other auxiliary agent in parts by weight, wherein the polar auxiliary agent is a composite of polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene.
2. The flame-free polypropylene material of claim 1, wherein the polypropylene is at least one of block co-polypropylene and homo-polypropylene, and the polypropylene has a melt flow rate of 1-100g/10min at 230 ℃/2.16KG test conditions.
3. The flame-free polypropylene material of claim 1, wherein the inorganic filler is at least one of talc, calcium carbonate, wollastonite, mica, and barium sulfate, and the particle size of the inorganic filler is 1 to 10 μm.
4. The flame free polypropylene material of claim 1, wherein the toughening agent is at least one of ethylene-butene copolymer and ethylene-octene copolymer, and the toughening agent has a density of 0.88 to 0.90g/cm3The melt flow rate at 190 ℃/2.16KG is 0.5-30g/10 min.
5. The flame free polypropylene material of claim 1, wherein the antioxidant comprises a primary antioxidant selected from hindered phenolic or thioester antioxidants and a secondary antioxidant selected from phosphite or ester antioxidants.
6. The flame free polypropylene material of claim 1, wherein the other additives comprise at least one of low molecular weight esters, metal soaps, complex esters of stearic acid.
7. The flame-free polypropylene material as claimed in claim 1, wherein the polypropylene-maleic acid alternating copolymer has a number average molecular weight of 1000-2500, an acid value of 30-60, and a structural formula:
8. the flame-free polypropylene material of claim 1, wherein the polar aid is a mixture of polypropylene-maleic acid alternating copolymer and acrylic acid grafted polypropylene, wherein the weight ratio of the polypropylene-maleic acid alternating copolymer in the polar aid is 20-80%.
9. A process for the preparation of a flame free polypropylene material according to any of claims 1 to 8, comprising the steps of:
fully mixing polypropylene, inorganic filler, toughening agent, polar additive, antioxidant and other additives according to a ratio to obtain a uniform mixed material;
and adding the mixed material into a double-screw extruder, and carrying out melting, extrusion, grain cutting and drying to obtain granules. Wherein the temperature of a material cylinder of the double-screw extruder is 190-230 ℃, the rotating speed of a screw is 400-450r/min, the rotating speed of a main machine is 18-20Hz, and the vacuum degree is-0.07-0.08 MPa.
10. Use of the flame retardant treated polypropylene material according to any one of claims 1 to 8 for the preparation of automotive interior trim parts.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112679861A (en) * | 2020-12-15 | 2021-04-20 | 江苏金发科技新材料有限公司 | Flame-treatment-free polypropylene composition for automobile bumpers and preparation method thereof |
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