CN110835442B - Polypropylene/polyamide/polyketone composite material and preparation method thereof - Google Patents

Polypropylene/polyamide/polyketone composite material and preparation method thereof Download PDF

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CN110835442B
CN110835442B CN201911269596.4A CN201911269596A CN110835442B CN 110835442 B CN110835442 B CN 110835442B CN 201911269596 A CN201911269596 A CN 201911269596A CN 110835442 B CN110835442 B CN 110835442B
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polypropylene
polyamide
resin
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CN110835442A (en
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李白羽
罗贤祖
韩春春
蓝承东
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Guangdong Aldex New Material Co Ltd
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Guangdong Aldex New Material Co Ltd
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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
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
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    • B29B7/28—Component parts, details or accessories; Auxiliary operations for measuring, controlling or regulating, e.g. viscosity control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/02—Making granules by dividing preformed material
    • B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/14—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the particular extruding conditions, e.g. in a modified atmosphere or by using vibration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
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    • B29C48/50—Details of extruders
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
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    • B29C48/505—Screws
    • B29C48/625—Screws characterised by the ratio of the threaded length of the screw to its outside diameter [L/D ratio]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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    • C08L2205/00—Polymer mixtures characterised by other features
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Abstract

The invention provides a polypropylene/polyamide/polyketone composite material and a preparation method thereof, wherein the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials: polypropylene resin, polyamide resin, polyketone resin, compatilizer, antioxidant, lubricant and metal toner master batch; the compatilizer is at least one of maleic anhydride grafted polypropylene and maleic anhydride grafted polyethylene; the metal toner master batch is prepared from metal toner, polyacrylic acid and polypropylene powder. The polypropylene/polyamide/polyketone composite material has high metal texture, excellent surface scratch resistance and good mechanical property, and can be applied to the fields of automobiles and household appliances such as automobile exterior decorations, air conditioner decorative strips, small household appliance exterior decorative structures and the like.

Description

Polypropylene/polyamide/polyketone composite material and preparation method thereof
Technical Field
The invention belongs to the field of materials, and particularly relates to a polypropylene/polyamide/polyketone composite material and a preparation method thereof.
Background
In recent years, with the development of coating-free materials, more and more parts are sprayed with paint and oil from the prior art, and the coating-free technology is adopted. The spray-free technique is generally to add metallic toner to a base resin to give a metallic texture to the obtained spray-free material. The spraying-free technology can save the process steps, reduce the cost and simultaneously protect the environment.
However, in practical use, the polypropylene spray-free material also faces a plurality of challenges, firstly, the metal toner is directly added into the resin, and the compatibility of the metal toner and the resin matrix is not good, so that ideal color and luster degree and high metal texture cannot be obtained; secondly, the scratch resistance of the resin matrix is poor, so that the spraying-free material is easy to scratch. For example, in the highlight non-spraying material of small household appliances, touch extrusion is inevitable to occur in the transportation process, the problem that scratches occur in the appearance due to the wiping of surface dust in the use process is likely to occur, the use experience of consumers can be greatly reduced due to the scratches, and the actual service life of related materials can also be shortened. Therefore, the metal texture and the scraping resistance of the polypropylene spraying-free material are improved while good mechanical properties are ensured, and the polypropylene spraying-free material has important practical significance.
Disclosure of Invention
Based on the above, the invention aims to provide a polypropylene/polyamide/polyketone composite material which has high metal texture, excellent surface scratch resistance and good mechanical properties, and can be applied to the fields of automobiles and household appliances such as automobile exterior decorations, air conditioner decorative strips and small household appliance exterior decorative structures.
The specific technical scheme is as follows:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
55-75 parts of polypropylene resin;
5-20 parts of polyamide resin;
10-30 parts of polyketone resin;
the sum of the parts by weight of the polypropylene resin, the polyamide resin and the polyketone resin is 100 parts;
Figure BDA0002313793970000021
the compatilizer is at least one of maleic anhydride grafted polypropylene and maleic anhydride grafted polyethylene;
the metal toner master batch is prepared from metal toner, polyacrylic acid and polypropylene powder.
Preferably, the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
60-75 parts of polypropylene resin;
10-15 parts of polyamide resin;
15-25 parts of polyketone resin;
the sum of the parts by weight of the polypropylene resin, the polyamide resin and the polyketone resin is 100 parts;
Figure BDA0002313793970000022
preferably, the metal toner master batch is prepared from metal toner, polyacrylic acid and polypropylene powder; wherein the mass ratio of the metallic toner to the polyacrylic acid is 1:1-10, more preferably 1:4-6, and more preferably 1: 5; the mass ratio of the total mass of the metal toner and the polyacrylic acid to the polypropylene powder is 1: 0.8-4; more preferably 1:0.8-1.2, still more preferably 1: 1.
Preferably, the metallic toner is at least one of aluminum powder, copper powder, gold powder, silver powder, zinc powder, tin powder, iron powder and nickel powder.
Preferably, the polyacrylic acid has a weight average molecular weight of 5000-50000; more preferably 10000-. More preferably 30000.
Preferably, the polypropylene powder has an average particle size of 0.01 to 10mm, more preferably 0.8 to 1.2 mm.
Preferably, the preparation method of the metal toner masterbatch comprises the following steps:
1) mixing the metallic toner with the polyacrylic acid;
2) mixing the mixed material obtained in the step 1) with the polypropylene powder;
3) and (3) melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extruder to obtain the metal toner master batch.
Preferably, the preparation method of the metal toner masterbatch comprises the following steps:
1) mixing the metal toner and the polyacrylic acid by using a stirrer, wherein the rotating speed of the stirrer is 100-300r/min, and the mixing time is 1-3 min;
2) mixing the mixed material obtained in the step 1) with the polypropylene powder by using a stirrer, wherein the rotating speed of the stirrer is 100-300r/min, and the mixing time is 1-3 min;
3) melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extruder to obtain the metal toner master batch; the technological parameters comprise: the temperature of the first zone is 150-170 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 190-210 ℃, the temperature of the fourth zone is 200-220 ℃, the temperature of the fifth zone is 200-220 ℃, the temperature of the sixth zone is 190-210 ℃, the temperature of the seventh zone is 190-210 ℃, the temperature of the eighth zone is 200-220 ℃, the temperature of the die head is 200-220 ℃, the rotating speed of the screw is 200-500 rpm, and the vacuum degree is-0.05-0.08 MPa; the ratio L/D of the length L and the diameter D of the screw of the double-screw extruder is 35-50; the screw is provided with 1-2 meshing block areas and 1-2 reverse thread areas.
Preferably, the melt index of the polypropylene resin under the condition of 230 ℃/2.16kg is 10-30g/10 min; more preferably, the melt index of the polypropylene resin under the condition of 230 ℃/2.16kg is 15-25g/10 min; further preferably, the polypropylene resin has a melt index of 20g/10min at 230 ℃/2.16 kg.
Preferably, the polyamide resin is polyamide 6; the relative viscosity of the polyamide 6 is 2-5; more preferably, the relative viscosity of said polyamide 6 is between 2.5 and 3.5; further preferably, the relative viscosity of the polyamide 6 is 3.
Preferably, the melt index of the polyketone resin at 230 ℃/2.16kg is 1-20g/10 min; more preferably, the melt index of the polyketone resin at 230 ℃/2.16kg is 3-15g/10 min; further preferably, the melt index of the polyketone resin is 10g/10min at 230 ℃/2.16 kg.
Preferably, the antioxidant is at least one of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid N-octadecyl ester, tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) phosphite. The antioxidant improves the processing stability of matrix resin in the processing process of the polypropylene/polyamide/polyketone composite material, and avoids the problems of material degradation and the like caused in the high-temperature processing process, thereby improving the overall performance of the material.
Preferably, the lubricant is at least one of silicone powder, calcium stearate and zinc stearate. The lubricant has good thermal stability and is not easy to decompose in the processing process of the polypropylene/polyamide/polyketone composite material. Meanwhile, in order to improve the processability of the material and reduce the comprehensive energy consumption by considering the high viscosity of the polyamide resin in the formula, a lubricant is introduced, and the certain amount of the lubricant can obviously reduce the torque of the material in the processing process.
Another object of the present invention is to provide a process for preparing a polypropylene/polyamide/polyketone composite material.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
mixing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant by using a stirrer, and adding the obtained mixed material into a double-screw extruder through a main feeder; adding the metal toner master batch into a double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch;
the technological parameters of the double-screw extruder comprise: the temperature of the first zone is 150-170 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 190-210 ℃, the temperature of the fourth zone is 200-220 ℃, the temperature of the fifth zone is 200-220 ℃, the temperature of the sixth zone is 190-210 ℃, the temperature of the seventh zone is 210-230 ℃, the temperature of the eighth zone is 210-240 ℃, the temperature of the die head is 210-240 ℃, the rotating speed of the screw is 200-500 rpm, and the vacuum degree is-0.05-0.08 MPa.
Preferably, the process parameters of the twin-screw extruder include: the temperature of the first zone is 160-170 ℃, the temperature of the second zone is 200-210 ℃, the temperature of the third zone is 200-210 ℃, the temperature of the fourth zone is 210-220 ℃, the temperature of the fifth zone is 210-220 ℃, the temperature of the sixth zone is 200-210 ℃, the temperature of the seventh zone is 220-230 ℃, the temperature of the eighth zone is 220-240 ℃, the temperature of the die head is 220-240 ℃, the rotating speed of the screw is 300-400 rpm, and the vacuum degree is-0.06-0.07 MPa.
Preferably, the ratio L/D of the length L and the diameter D of the screw of the parallel double-screw extruder is 35-50; the screw is provided with 1-2 meshing block areas and 1-2 reverse thread areas.
Preferably, the mixing is carried out in a high-speed stirrer, and the rotating speed of the high-speed stirrer is 500-1200 rpm; more preferably, the rotating speed of the high-speed stirrer is 700 and 1000 revolutions per minute.
The principle of the polypropylene-polyamide-polyketone composite material of the invention is as follows:
the invention takes polypropylene, polyamide and polyketone as matrix resin, and prepares the polymer composite material with high metal texture, excellent wear resistance and excellent mechanical property by matching with a certain amount of specific compatilizer and specific metal toner master batch.
After a specific kind of compatilizer is introduced, one end of the compatilizer is a non-polar structure, the other end of the compatilizer is a polar structure, for example, maleic anhydride grafted polypropylene is taken as an example, one end of the compatilizer is polypropylene with a non-polar structure, the molecular structure of the compatilizer is similar to that of polypropylene, the compatilizer has good physical compatibility with polypropylene, and the other end of the compatilizer is maleic anhydride. In addition, due to the interaction of the molecules of the polyamide and the polyketone in the phase interface nano scale, the two polymers can obtain good compatibility by physical blending without any chemical reaction, so that the compatibility of the polypropylene, the polyketone and the polyamide can be greatly improved by adding the polyamide and matching with a proper amount of a specific kind of compatilizer, thereby obtaining a polypropylene-nylon-polyketone three-component composite material with better compatibility, and the composite material has excellent mechanical property and wear resistance. On the basis, the specific metal toner master batch is added, the metal toner master batch is pretreated by polyacrylic acid firstly, and then the metal toner master batch and polypropylene are prepared into master batches, so that the compatibility of the metal toner and a polypropylene/polyamide/polyketone three-component polymer is obviously improved while the metal texture and the gloss are not influenced, the dispersity of the metal toner in a polymer material is greatly improved, the material can have strong metal texture under the condition of only using a small amount of the metal toner, and the metal toner master batch has excellent mechanical properties.
Therefore, the invention has the following beneficial effects:
the polypropylene/polyamide/polyketone composite material disclosed by the invention is obvious in spraying-free effect, high in metal texture and glossiness, excellent in mechanical property and scraping resistance, capable of being applied to the kitchen electric field such as an electric cooker shell and an electric pressure cooker shell, and capable of being expanded to be used in the fields of automobile exterior decorations, air conditioner decorative strips, other small household appliance exterior decorations and the like.
The preparation method of the polypropylene/polyamide/polyketone composite material provided by the invention has the advantages of simple preparation process, easiness in control, low requirement on equipment, low investment and contribution to industrial production, and all used equipment is general processing equipment.
Drawings
FIG. 1 is a flow chart of a preparation process of a polypropylene-polyamide-polyketone composite material according to an embodiment of the present invention;
FIG. 2 is a diagram of an actual article of polypropylene-polyamide-polyketone composite material according to example 7 of the present invention.
Detailed Description
In order that the invention may be more readily understood, reference will now be made to the following more particular description of the invention, examples of which are set forth below. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. These embodiments are provided so that this disclosure will be thorough and complete. It is to be understood that the experimental procedures in the following examples, where specific conditions are not noted, are generally in accordance with conventional conditions, or with conditions recommended by the manufacturer. The various reagents used in the examples are commercially available.
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 in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The raw material components and sources thereof used in the specific embodiment of the present invention are as follows:
polypropylene resin with a melt index of 20g/10min at 230 ℃/2.16kg, selected from China petrochemical group Michelson petrochemical company Limited;
polyamide 6 resin with relative viscosity of 3, selected from Henan Shenma Nylon chemical Limited liability company;
a polyketone resin having a melt index of 10g/10min selected from the group consisting of Xiaoxing, Korea;
a compatilizer: maleic anhydride grafted polypropylene selected from Shenyang Ketong, Inc.;
antioxidant: n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], selected from Beijing very easily available chemical Co., Ltd;
antioxidant: n, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) phosphite selected from Beijing Tiangang auxiliary agent, Limited liability company;
A lubricant silicone powder selected from Chuanzhuighua chemical engineering Co., Ltd., Guangzhou;
a lubricant of calcium stearate and a lubricant of zinc stearate, which are selected from Zichuan Ruifeng plastics auxiliaries;
metallic toner: aluminum powder and silver powder selected from the plastics industries of New color Yan, Shunde district, Fushan;
polyacrylic acid (weight average molecular weight 10000, 30000, 50000) selected from sigma aldrich trade ltd;
polypropylene powder selected from south China division of China petrochemical industry sales Limited;
the metal toner master batch is self-made.
The present invention will be described in detail with reference to specific examples.
Example 1
The polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000071
antioxidant: 0.5 part of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester;
0.5 part of lubricant calcium stearate;
and 3 parts of metal toner master batch.
The preparation method of the metal toner master batch comprises the following steps:
1) mixing metal toner aluminum powder and polyacrylic acid with the weight-average molecular weight of 10000 by a stirrer according to the mass ratio of 1:10, wherein the rotating speed of the stirrer is 100r/min, and the mixing time is 1 min;
2) Adding polypropylene powder with the average particle size of 0.01mm into the mixture obtained in the step 1), wherein the mass ratio of the polypropylene powder to the total mass of the mixture obtained in the step 1) is 1:1, and continuously mixing the mixture by using a stirrer, wherein the rotating speed of the stirrer is 100r/min, and the mixing time is 1 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 150 ℃, the temperature of the second zone is 190 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 200 ℃, the temperature of the fifth zone is 200 ℃, the temperature of the sixth zone is 190 ℃, the temperature of the seventh zone is 190 ℃, the temperature of the eighth zone is 200 ℃, the temperature of the die head is 200 ℃, the rotating speed of the screw is 200rpm, the vacuum degree is-0.05 MPa, the ratio L/D of the length L and the diameter D of the screw is 35, and the screw is provided with 1 meshing block zone and 1 back thread zone.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant in parts by weight, and mixing by using a high-speed stirrer at 500 revolutions per minute.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 150 ℃, the temperature of the second zone is 190 ℃, the temperature of the third zone is 190 ℃, the temperature of the fourth zone is 200 ℃, the temperature of the fifth zone is 200 ℃, the temperature of the sixth zone is 190 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 200rpm, the vacuum degree is-0.05 MPa, the ratio L/D of the length L and the diameter D of the screw is 35, and the screw is provided with 1 meshing block zone and 1 reverse thread zone.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 2
The polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000081
Figure BDA0002313793970000091
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 10mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 800 revolutions per minute.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 230 ℃, the temperature of the eighth zone is 240 ℃, the temperature of the die head is 240 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 3:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000101
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 50000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 4:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000111
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 5:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000121
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 6:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000131
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Example 7:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000141
Figure BDA0002313793970000151
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the polypropylene powder to the total mass of the mixture obtained in the step 1) is 1:1, and continuously mixing the mixture by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone was 160 ℃, the temperature of the second zone was 200 ℃, the temperature of the third zone was 200 ℃, the temperature of the fourth zone was 210 ℃, the temperature of the fifth zone was 210 ℃, the temperature of the sixth zone was 200 ℃, the temperature of the seventh zone was 200 ℃, the temperature of the eighth zone was 210 ℃, the temperature of the die head was 210 ℃, the rotation speed of the screw was 300rpm, and the vacuum was-0.06 MPa. The ratio L/D of the length L of the screw rod and the diameter D of the screw rod is 45, and the screw rod is provided with 1 meshing block area and 2 reverse thread areas.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1000 revolutions per minute.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 350rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 reverse thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
The polypropylene/polyamide/polyketone composite material obtained in the embodiment is subjected to injection molding according to a conventional method to obtain an article product shown in fig. 2, and as can be seen from fig. 2, the article product has good appearance and a spraying-free effect.
Example 8
The polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000161
the preparation method of the metal toner master batch comprises the following steps:
1) Mixing metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone was 160 ℃, the temperature of the second zone was 200 ℃, the temperature of the third zone was 200 ℃, the temperature of the fourth zone was 210 ℃, the temperature of the fifth zone was 210 ℃, the temperature of the sixth zone was 200 ℃, the temperature of the seventh zone was 200 ℃, the temperature of the eighth zone was 210 ℃, the temperature of the die head was 210 ℃, the rotation speed of the screw was 300rpm, and the vacuum was-0.06 MPa. The ratio L/D of the length L of the screw rod and the diameter D of the screw rod is 45, and the screw rod is provided with 1 meshing block area and 2 reverse thread areas.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) Weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant in parts by weight, and mixing by using a high-speed stirrer at 1000 rpm.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 350rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 1:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000171
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 2:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000181
Figure BDA0002313793970000191
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the polypropylene powder to the total mass of the mixture obtained in the step 1) is 1:1, and continuously mixing the mixture by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 3:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000201
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 4:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000211
the preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixture mixed in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner into the side of the parallel double-screw extruder (total eight zones) for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 5:
the polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000221
the preparation method of the untreated metal toner master batch comprises the following steps:
1) mixing the metal toner and polypropylene powder with the average particle size of 1mm by using a stirrer, wherein the mass ratio is 1:1, the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) Adding the mixed material obtained in the step 1) into a double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the untreated metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone is 160 ℃, the temperature of the second zone is 200 ℃, the temperature of the third zone is 200 ℃, the temperature of the fourth zone is 210 ℃, the temperature of the fifth zone is 210 ℃, the temperature of the sixth zone is 200 ℃, the temperature of the seventh zone is 200 ℃, the temperature of the eighth zone is 210 ℃, the temperature of the die head is 210 ℃, the rotating speed of the screw is 300rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 45, and the screw is provided with 1 meshing block zone and 2 reverse thread zones.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant according to the parts by weight, and mixing by using a high-speed stirrer at 1200 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding untreated metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 210 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 500rpm, the vacuum degree is-0.08 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
Comparative example 6
The polypropylene/polyamide/polyketone composite material is prepared from the following raw materials in parts by weight:
Figure BDA0002313793970000231
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metal toner silver powder and polyacrylic acid with the weight-average molecular weight of 30000 according to the mass ratio of 1:5 by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
2) adding polypropylene powder with the average particle size of 1mm into the mixture obtained in the step 1), wherein the mass ratio of the total mass of the mixture obtained in the step 1) to the mass of the polypropylene powder is 1:1, and continuously mixing by using a stirrer, wherein the rotating speed of the stirrer is 200r/min, and the mixing time is 2 min;
3) and (3) adding the mixed material obtained in the step 2) into a parallel double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch. The technological parameters of the parallel double-screw extruder for melt extrusion and granulation are as follows: the temperature of the first zone was 160 ℃, the temperature of the second zone was 200 ℃, the temperature of the third zone was 200 ℃, the temperature of the fourth zone was 210 ℃, the temperature of the fifth zone was 210 ℃, the temperature of the sixth zone was 200 ℃, the temperature of the seventh zone was 200 ℃, the temperature of the eighth zone was 210 ℃, the temperature of the die head was 210 ℃, the rotation speed of the screw was 300rpm, and the vacuum was-0.06 MPa. The ratio L/D of the length L of the screw rod and the diameter D of the screw rod is 45, and the screw rod is provided with 1 meshing block area and 2 reverse thread areas.
The preparation method of the polypropylene/polyamide/polyketone composite material comprises the following steps:
1) weighing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant in parts by weight, and mixing by using a high-speed stirrer at 1000 rpm.
2) Adding the mixed material obtained in the step 1) into a parallel double-screw extruder through a main feeder, adding metal toner master batches into the parallel double-screw extruder (total eight zones) in the lateral direction for melt extrusion, and granulating, wherein the process parameters are as follows: the temperature of the first zone is 170 ℃, the temperature of the second zone is 210 ℃, the temperature of the third zone is 210 ℃, the temperature of the fourth zone is 220 ℃, the temperature of the fifth zone is 220 ℃, the temperature of the sixth zone is 210 ℃, the temperature of the seventh zone is 220 ℃, the temperature of the eighth zone is 220 ℃, the temperature of the die head is 220 ℃, the rotating speed of the screw is 350rpm, the vacuum degree is-0.06 MPa, the ratio L/D of the length L and the diameter D of the screw is 50, and the screw is provided with 2 meshing block zones and 2 back thread zones.
And carrying out melt extrusion and granulation by a parallel double-screw extruder under the process conditions to obtain the granular polypropylene/polyamide/polyketone composite material.
The following is a list of raw material compositions of examples and comparative examples (table 1).
TABLE 1 summary of the composition parts by weight of the raw materials of the examples and comparative examples
Figure BDA0002313793970000241
The polypropylene/polyamide/polyketone composites prepared in the above examples and comparative examples were subjected to the following performance tests:
tensile property: testing according to GB/T1040-2006 standard, wherein the stretching speed is 50 mm/min;
bending property: according to the test of GB/T9341-;
gloss: testing according to GB/T8807-1988 standard, selecting a 60-degree angle in the test, wherein the higher the glossiness of the material is, the stronger the texture of the material is, and the better the spraying-free effect is;
scratch resistance: according to the GMW 14688-.
The results of the performance tests are shown in table 2.
TABLE 2 Properties of Polypropylene/Polyamide/polyketone composites for the examples and comparative examples
Figure BDA0002313793970000251
In examples 1 to 8, the proportions of the polypropylene resin, the polyamide resin, the polyketone resin, the compatibilizer, the antioxidant, the lubricant, and the metallic toner masterbatch were adjusted, and it can be seen from the table that, when the content of the polypropylene resin is decreased (the content of the polyamide resin and the content of the polyketone resin are increased) within a certain range, the tensile strength and the flexural strength of the polypropylene/polyamide/polyketone composition composite material are slightly increased, but the impact on the glossiness and the scratch resistance is not great. Within a certain range, the increase or decrease of the compatilizer has little influence on the mechanical property of the system, and the change of the contents of the antioxidant and the lubricant has little influence on the mechanical property of the system. With the increase of the addition amount of the metal toner master batch, the surface gloss of the polypropylene/polyamide/polyketone composition composite material is remarkably improved, but when the addition amount exceeds 5 parts, the influence of the addition amount of the metal toner master batch on the gloss is not large. The reason is that the influence of the metallic toner on the glossiness of the material is mainly provided by the distribution of the metallic toner on the surface of the material, if the metallic toner structure on the surface of the material tends to be saturated, the addition of the metallic toner masterbatch does not further contribute to the glossiness, and the production price of the metallic toner masterbatch is relatively high. By comparison, the overall performance of example 7 is best.
Comparative examples 1 and 2 compared to example 7, comparative examples 1 and 2 used less polyamide and polyketone resin, respectively, and the resulting polypropylene/polyamide/polyketone composites all had a significant decrease in tensile strength, flexural strength and scratch resistance; comparative example 3 compared with example 7, the polypropylene/polyamide/polyketone composite material obtained by using too little compatilizer in comparative example 3 has obviously reduced overall mechanical properties, because the polypropylene/polyamide/polyketone composite material has obvious phase separation due to too little compatilizer, the material is easy to generate defects at the edges of the phase, and the defects are more easily converted into cracks under stress, so that the material has reduced properties. Comparative example 4 in comparison with example 7, comparative example 4 directly used a metal toner in an amount slightly larger than the content of the metal toner in the mother particle of example 7. The metallic toner of comparative example 4 has poor compatibility with the resin and poor dispersion in the resin because it is not pretreated, resulting in much lower gloss of the resulting polypropylene/polyamide/polyketone composite than that of example 7. Comparative example 5 compared with example 7, comparative example 5 directly used the untreated metallic toner mother particle, and the gloss of the resulting polypropylene/polyamide/polyketone composite was far less excellent than that of example 7, although better than that of comparative example 4. The result shows that the treatment of the polyacrylic acid on the metal toner and the preparation of the master batch can synergistically improve the interface compatibility of the metal toner and the matrix resin, so that the metal toner is better dispersed in the resin, and the glossiness is improved to a greater extent. Comparative example 6 has a significantly reduced content of polypropylene compared to example 7, resulting in a significant deterioration of the mechanical properties of the resulting polypropylene/polyamide/polyketone composite, mainly due to the transformation of the matrix of the ternary blend system, and increasing the content of polyamide and polyketone would instead lead to problems of compatibility between the resins, further resulting in a significant reduction of the overall mechanical properties of the polypropylene/polyamide/polyketone composite.
The technical features of the above embodiments can be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the above embodiments are not described, however, as long as there is no contradiction between the combinations of the technical features, the scope of the present description should be considered as being described in the present specification.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the present 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 polypropylene/polyamide/polyketone composite material is characterized by being prepared from the following raw materials in parts by weight:
55-75 parts of polypropylene resin;
5-20 parts of polyamide resin;
10-30 parts of polyketone resin;
the sum of the parts by weight of the polypropylene resin, the polyamide resin and the polyketone resin is 100 parts;
Figure FDA0003530483160000011
the compatilizer is at least one of maleic anhydride grafted polypropylene and maleic anhydride grafted polyethylene;
The metal toner master batch is prepared from metal toner, polyacrylic acid and polypropylene powder;
the preparation method of the metal toner master batch comprises the following steps:
1) mixing the metallic toner with the polyacrylic acid;
2) mixing the mixed material obtained in the step 1) with the polypropylene powder;
3) and (3) melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extruder to obtain the metal toner master batch.
2. The polypropylene/polyamide/polyketone composite material as claimed in claim 1, which is prepared from the following raw materials in parts by weight:
60-75 parts of polypropylene resin;
10-15 parts of polyamide resin;
15-25 parts of polyketone resin;
the sum of the parts by weight of the polypropylene resin, the polyamide resin and the polyketone resin is 100 parts;
Figure FDA0003530483160000012
Figure FDA0003530483160000021
3. the polypropylene/polyamide/polyketone composite material according to claim 1, wherein the metallic toner masterbatch is prepared from metallic toner, polyacrylic acid and polypropylene powder; wherein the mass ratio of the metallic toner to the polyacrylic acid is 1: 1-10; the mass ratio of the total mass of the metal toner and the polyacrylic acid to the polypropylene powder is 1: 0.8-4.
4. The polypropylene/polyamide/polyketone composite material according to claim 3, wherein the metal toner masterbatch is prepared from a metal toner, polyacrylic acid and a polypropylene powder; wherein the mass ratio of the metal toner to the polyacrylic acid is 1: 4-6; the mass ratio of the total mass of the metal toner and the polyacrylic acid to the polypropylene powder is 1: 0.8-1.2.
5. The polypropylene/polyamide/polyketone composite material according to claim 1, wherein the metallic toner is at least one of aluminum powder, copper powder, gold powder, silver powder, zinc powder, tin powder, iron powder, and nickel powder; and/or the like, and/or,
the weight average molecular weight of the polyacrylic acid is 5000-50000; and/or the like, and/or,
the average grain diameter of the polypropylene powder is 0.01-10 mm.
6. The polypropylene/polyamide/polyketone composite material according to claim 1, wherein the preparation method of the metallic toner masterbatch comprises the steps of:
1) mixing the metal toner and the polyacrylic acid by using a stirrer, wherein the rotating speed of the stirrer is 100-300r/min, and the mixing time is 1-3 min;
2) mixing the mixed material obtained in the step 1) with the polypropylene powder by using a stirrer, wherein the rotating speed of the stirrer is 100-300r/min, and the mixing time is 1-3 min;
3) Melting, extruding and granulating the mixed material obtained in the step 2) by using a double-screw extruder to obtain the metal toner master batch; the technological parameters comprise: the temperature of the first zone is 150-170 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 190-210 ℃, the temperature of the fourth zone is 200-220 ℃, the temperature of the fifth zone is 200-220 ℃, the temperature of the sixth zone is 190-210 ℃, the temperature of the seventh zone is 190-210 ℃, the temperature of the eighth zone is 200-220 ℃, the temperature of the die head is 200-220 ℃, the rotating speed of the screw is 200-500 rpm, and the vacuum degree is-0.05-0.08 MPa; the ratio L/D of the length L and the diameter D of the screw of the double-screw extruder is 35-50; the screw is provided with 1-2 meshing block areas and 1-2 reverse thread areas.
7. The polypropylene/polyamide/polyketone composite material according to any one of claims 1 to 6, wherein the polypropylene resin has a melt index of 10 to 30g/10min at 230 ℃/2.16 kg; and/or the like, and/or,
the polyamide resin is polyamide 6, and the relative viscosity of the polyamide 6 is 2-5; and/or the presence of a catalyst in the reaction mixture,
the melt index of the polyketone resin under the condition of 230 ℃/2.16kg is 1-20g/10 min.
8. The polypropylene/polyamide/polyketone composite material according to any one of claims 1 to 6, wherein the antioxidant is at least one of N-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) phosphite; and/or the presence of a catalyst in the reaction mixture,
The lubricant is at least one of silicone powder, calcium stearate and zinc stearate.
9. A process for the preparation of a polypropylene/polyamide/polyketone composite material according to any one of claims 1 to 8, characterized in that it comprises the following steps:
mixing the polypropylene resin, the polyamide resin, the polyketone resin, the compatilizer, the antioxidant and the lubricant by using a stirrer, and adding the obtained mixed material into a double-screw extruder through a main feeder; adding the metal toner master batch into a double-screw extruder through a side feeder, and then carrying out melt extrusion and granulation to obtain the metal toner master batch;
the technological parameters of the double-screw extruder comprise: the temperature of the first zone is 150-170 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 190-210 ℃, the temperature of the fourth zone is 200-220 ℃, the temperature of the fifth zone is 200-220 ℃, the temperature of the sixth zone is 190-210 ℃, the temperature of the seventh zone is 210-230 ℃, the temperature of the eighth zone is 210-240 ℃, the temperature of the die head is 210-240 ℃, the rotating speed of the screw is 200-500 rpm, and the vacuum degree is-0.05-0.08 MPa.
10. The process for the preparation of polypropylene/polyamide/polyketone composites according to claim 9, wherein the process parameters of the twin-screw extruder comprise: the temperature of the first zone is 160-170 ℃, the temperature of the second zone is 200-210 ℃, the temperature of the third zone is 200-210 ℃, the temperature of the fourth zone is 210-220 ℃, the temperature of the fifth zone is 210-220 ℃, the temperature of the sixth zone is 200-210 ℃, the temperature of the seventh zone is 220-230 ℃, the temperature of the eighth zone is 220-240 ℃, the temperature of the die head is 220-240 ℃, the rotating speed of the screw is 300-400 rpm, and the vacuum degree is-0.06-0.07 MPa; and/or the presence of a catalyst in the reaction mixture,
The ratio L/D of the length L and the diameter D of the screw of the double-screw extruder is 35-50; the screw is provided with 1-2 meshing block areas and 1-2 reverse thread areas.
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