CN107501716B - Polypropylene filling master batch prepared from polypropylene reclaimed material and preparation method thereof - Google Patents

Polypropylene filling master batch prepared from polypropylene reclaimed material and preparation method thereof Download PDF

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CN107501716B
CN107501716B CN201610426003.0A CN201610426003A CN107501716B CN 107501716 B CN107501716 B CN 107501716B CN 201610426003 A CN201610426003 A CN 201610426003A CN 107501716 B CN107501716 B CN 107501716B
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polypropylene
temperature
parts
master batch
filling master
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CN107501716A (en
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杨桂生
方永炜
梁娜
朱敏
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CHUZHOU GENIUS NEW MATERIALS Co.,Ltd.
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Hefei Genius New Materials Co Ltd
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
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    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
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    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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    • C08J2423/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/20Recycled plastic

Abstract

The invention discloses a polypropylene filling master batch prepared from a polypropylene reclaimed material and a preparation method thereof, wherein the polypropylene filling master batch is prepared from the following components in parts by weight: polypropylene reclaimed materials, low-density polyethylene, polypropylene grafted acrylic acid, inorganic mineral filler, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, an antioxidant and a lubricant. The invention solves the problems of high cost, poor dispersibility, poor compatibility and the like of the conventional filling master batch in the current market, and expands the application range of the recycled plastic. The filling master batch processed by the invention is widely used for filling modification of materials such as automobiles, pipelines, cables and the like, can greatly modify raw materials under the condition of meeting the product performance requirement, reduce the cost and improve the use value of the recycled plastics.

Description

Polypropylene filling master batch prepared from polypropylene reclaimed material and preparation method thereof
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to a polypropylene filling master batch prepared from a polypropylene reclaimed material and a preparation method thereof.
Background
In order to enhance the relevant properties of the plastic material, such as mechanical property, density and the like, the plastic material is generally modified by adding some modifiers, powder is directly used in the aspect of filling modification at first in the plastic modification, and the modification mode has great pollution to the production environment on one hand, and the powder is poor in dispersion on the other hand, so that the final product performance is influenced. In recent years, with the continuous update and development of plastic modification technology, the filling master batch used for filling modification becomes a production form of many enterprises, and the pollution and processing technology are effectively improved.
At present, the base materials mainly adopted by a large amount of filling master batches in the market are new materials such as polypropylene, low-density polyethylene, polyolefin elastomer (POE) and the like, and the cost of the produced raw materials is higher. The filling master batch is produced by using the regenerated plastic as a base material and then matched with corresponding auxiliary agents, so that the raw material cost can be effectively reduced, the filling master batch with good dispersion performance and compatibility can be obtained, and the filling master batch can be widely used in the plastic modification industry, such as automobiles, pipelines, cables and the like.
Disclosure of Invention
The invention aims to provide a polymer filling master batch prepared from a polypropylene reclaimed material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: a polypropylene filling master batch prepared from a polypropylene reclaimed material is prepared from the following components in parts by weight:
the recycled polypropylene material is injection molding grade polypropylene which is prepared by sorting, cleaning, crushing and drying after being recycled, the water content of the recycled polypropylene material is lower than 0.5%, the combustion residue is less than 3%, and the melt index is 15-60g/10min under the condition of 2.16kg/230 ℃.
The low-density polyethylene has a melt index of 60g/10min at 230 ℃/2.16 Kg.
The grafting rate of the polypropylene grafted acrylic acid is more than or equal to 1.5 percent, and the weight average molecular weight is more than or equal to 20000.
The inorganic mineral filler is one or more of talcum powder, calcium carbonate or mica with the grain diameter of more than or equal to 3000 meshes.
The antioxidant is prepared by compounding tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (1010) and 6- (4-hydroxy-3, 5-di-tert-butylphenylamino) -2, 4-di-n-octylthio-1, 3, 5-triazine (antioxidant 565) according to the mass ratio of 1: 2.
The lubricant is prepared by compounding white mineral oil, Ethylene Bis Stearamide (EBS) and calcium stearate according to the mass ratio of 2:1: 1.
The invention also aims to provide a method for preparing the polypropylene filling master batch, which comprises the following steps:
(1) adding the dried polypropylene reclaimed material, low-density polyethylene, polypropylene grafted acrylic acid, an antioxidant and a lubricant into a temperature-controlled high-speed mixer according to the proportion and mixing for 2-3 min; the temperature of the mixer is 75-90 ℃, and the rotating speed is 500-800 r/min;
(2) adding an inorganic mineral filler into the mixture obtained in the step (1) for stirring, adding 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane at a constant speed in the stirring process, and continuously stirring and mixing for 10-15min to obtain a premix;
(3) putting the premix into a double-screw extruder with the length-diameter ratio of 44:1, preheating for 2-4 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of the double-screw extruder is set as follows: the temperature of the pre-melting zone is 140-155 ℃, the temperature of the first melting zone is 190-200 ℃, the temperature of the first high-temperature shearing zone is 200-210 ℃, the temperature of the second high-temperature shearing zone is 210-220 ℃, the temperature of the second melting zone is 200-210 ℃, and the temperature of the discharge hole is 190-200 ℃. The rotating speed of the double-screw extruder in the processing process is 300-500 rpm.
The polypropylene filling master batch prepared from the polypropylene reclaimed material is mixed with polypropylene according to a certain proportion, and then the mixture is melted and extruded to obtain the composite material, wherein the polypropylene filling master batch can obviously improve the tensile strength, the elongation at break, the bending strength, the bending modulus and the cantilever beam notch impact of the composite material and has better rigidity, toughness and strength compared with the proportion.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the polypropylene grafted acrylic acid is added into the polypropylene reclaimed material, so that a strong polar reactive group is introduced, and the material has high polarity and reactivity, thereby greatly improving the compatibility between the polypropylene and the mineral filler;
2. the 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane added in the invention and the polypropylene graft acrylic acid act together to change the hydrophilicity of the surface of the inorganic mineral filler into lipophilicity, so that the inorganic mineral filler is tightly combined with the polypropylene, the strength, the cohesive force, the dispersion performance and the like of the composite material are obviously improved, and the finally prepared master batch has good dispersibility and compatibility;
3. the purpose of adding the low-density polyethylene in the invention is to adjust the viscosity of the melt during melt extrusion, so that the melt is well dispersed and uniformly mixed, thereby solving the problems of strip breakage, a Du's plug die head and the like during extrusion.
4. The invention uses the special antioxidant compounded by the antioxidant 1010 and the antioxidant 565, the dosage of the special antioxidant is only 0.01 to 0.02 part, and the dosage of the common antioxidant is about 0.5 percent, thereby greatly reducing the dosage of the antioxidant; and can protect the material from thermal oxidative degradation during production, processing and final use, thereby well maintaining the mechanical properties of the composition.
5. The invention solves the problems of high cost, poor dispersibility, poor compatibility and the like of the conventional filling master batch in the current market, and expands the application range of the recycled plastic. The filling master batch processed by the invention is widely used for filling modification of materials such as automobiles, pipelines, cables and the like, can greatly modify raw materials under the condition of meeting the product performance requirement, reduce the cost and improve the use value of the recycled plastics.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting thereof.
The following examples used the raw materials:
the lubricant is prepared by compounding white mineral oil, Ethylene Bis Stearamide (EBS) and calcium stearate according to the mass ratio of 2:1: 1.
The antioxidant is compounded by an antioxidant 1010 and an antioxidant 565 according to the mass ratio of 1: 2.
The polypropylene return material is injection molding grade polypropylene which is prepared by sorting, cleaning, crushing and drying after recovery, the water content of the polypropylene return material is lower than 0.5 percent, the combustion residue is less than 3 percent, and the melt index is 15-60g/10min under the conditions of 2.16kg and 230 ℃.
Example 1
Putting 10 parts of dried polypropylene reclaimed materials, 5 parts of 10 parts of low-density polyethylene polypropylene grafted acrylic acid, 0.01 part of antioxidant and 1.6 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 2min, controlling the temperature at 80 ℃ and the rotating speed at 700 r/min;
then adding 85 parts of inorganic mineral filler calcium carbonate into a high-speed mixer, adding 1.7 parts of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 750r/min, and continuously stirring for 12min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder with the length-diameter ratio of 44:1, preheating for 3 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each area of the double-screw extruder is as follows: the temperature of the pre-melting zone is 140 ℃, the temperature of the first melting zone is 195 ℃, the temperature of the first high-temperature shearing zone is 205 ℃, the temperature of the second high-temperature shearing zone is 210 ℃, the temperature of the second melting zone is 205 ℃, the temperature of the melting zone at the discharge hole is 195 ℃, and the rotating speed of the screw is 350 rpm.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
Example 2
Putting 13 parts of dried polypropylene reclaimed materials, 30 parts of low-density polyethylene, 2 parts of polypropylene grafted acrylic acid, 0.02 part of antioxidant and 3 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 3min, controlling the temperature at 75 ℃ and rotating at the speed of 600 r/min;
then adding 55 parts of inorganic mineral filler calcium carbonate and 30 parts of talcum powder into a high-speed mixer, adding 0.4 part of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 650r/min, and continuously stirring for 15min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder, preheating for 2 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each zone of the double-screw extruder is as follows: 155 ℃ of a pre-melting zone, 200 ℃ of a first melting zone, 210 ℃ of a first high-temperature shearing zone, 220 ℃ of a second high-temperature shearing zone, 210 ℃ of a second melting temperature zone, 200 ℃ of a discharge port melting temperature zone and 400 rpm of a screw.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
Example 3
Putting 15 parts of dried polypropylene reclaimed materials, 20 parts of low-density polyethylene, 5 parts of polypropylene grafted acrylic acid, 0.01 part of antioxidant and 2.5 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 3min, controlling the temperature at 90 ℃ and rotating speed at 800 r/min;
then adding 35 parts of inorganic mineral filler mica powder and 45 parts of talcum powder into a high-speed mixer, adding 1 part of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 800r/min, and continuously stirring for 12min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder, preheating for 3 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each zone of the double-screw extruder is as follows: the temperature of the pre-melting zone is 140 ℃, the temperature of the first melting zone is 190 ℃, the temperature of the first high-temperature shearing zone is 200 ℃, the temperature of the second high-temperature shearing zone is 210 ℃, the temperature of the second melting zone is 200 ℃, the temperature of the melting zone of the discharge hole is 190 ℃, and the rotating speed of the screw is 300 rpm.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
Example 4
Putting 20 parts of dried polypropylene reclaimed materials, 20 parts of low-density polyethylene, 5 parts of polypropylene grafted acrylic acid, 0.01 part of antioxidant and 1.5 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 3min, controlling the temperature at 75 ℃ and the rotating speed at 600 r/min;
then adding 75 parts of inorganic mineral filler talcum powder into a high-speed mixer, adding 0.4 part of 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 500r/min, and continuously stirring for 10min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder, preheating for 2 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each zone of the double-screw extruder is as follows: the temperature of the pre-melting zone is 145 ℃, the temperature of the first melting zone is 200 ℃, the temperature of the first high-temperature shearing zone is 205 ℃, the temperature of the second high-temperature shearing zone is 215 ℃, the temperature of the second melting zone is 205 ℃, the temperature of the melting zone at the discharge hole is 195 ℃, and the rotating speed of the screw is 500 rpm.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
Example 5
Placing 16 parts of dried polypropylene reclaimed materials, 30 parts of low-density polyethylene, 4 parts of polypropylene grafted acrylic acid, 0.01 part of antioxidant and 2 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 2min, controlling the temperature at 90 ℃ and rotating at the speed of 500 r/min;
then adding 50 parts of inorganic mineral filler calcium carbonate and 30 parts of mica powder into a high-speed mixer, adding 1.6 parts of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 600r/min, and continuously stirring for 13min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder, preheating for 2 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each zone of the double-screw extruder is as follows: the temperature of the pre-melting zone is 150 ℃, the temperature of the first melting zone is 200 ℃, the temperature of the first high-temperature shearing zone is 205 ℃, the temperature of the second high-temperature shearing zone is 220 ℃, the temperature of the second melting zone is 205 ℃, the temperature of the melting zone at the discharge hole is 195 ℃, and the rotating speed of the screw is 450 rpm.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
Example 6
Putting 14 parts of dried polypropylene reclaimed materials, 10 parts of low-density polyethylene, 6 parts of polypropylene grafted acrylic acid, 0.01 part of antioxidant and 2.8 parts of lubricant into a temperature-controlled high-speed mixer for mixing for 3min, controlling the temperature at 85 ℃ and the rotating speed at 650 r/min;
then adding 80 parts of inorganic mineral filler mica powder into a high-speed mixer, adding 0.4 part of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed while stirring, controlling the rotating speed of the high-speed mixer at 550r/min, and continuously stirring for 14min after the addition is finished to obtain a premix;
and finally feeding the premix into a double-screw extruder, preheating for 4 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the filling master batch, wherein the temperature of each zone of the double-screw extruder is as follows: the temperature of the pre-melting zone is 145 ℃, the temperature of the first melting zone is 195 ℃, the temperature of the first high-temperature shearing zone is 210 ℃, the temperature of the second high-temperature shearing zone is 215 ℃, the temperature of the second melting zone is 200 ℃, the temperature of the melting zone of the discharge hole is 195 ℃, and the rotating speed of the screw is 400 rpm.
Mixing the prepared filling master batch and polypropylene according to the mass ratio of 25: 75, mixing, melting and extruding to obtain the composite material.
The composites prepared in examples 1-6 above were injection molded into bars with the properties shown in Table 1.
The polypropylene and the recycled material of the waste polypropylene washing machine cylinder (the water content is lower than 0.5%, the combustion residue is less than 3%, and the melt index is 15-60g/10min under the condition of 2.16Kg/230 ℃) with the melt index of 40-100 g/10min under the condition of 230 ℃ \2.16Kg are used as comparative examples, and the performance is tested by injection molding into sample strips in the same way, as shown in the following table 1.
The test methods of the physical properties are respectively as follows:
the melt flow rate was tested according to GB/T3682-;
the tensile strength and the elongation at break are measured according to GB/T1040.2-2006;
the bending strength and the bending modulus are measured according to GB/T9341-;
the notched impact strength of the cantilever beam is measured according to GB/T1834-2008;
the load deflection temperature was measured according to GB/T1634.2-2004;
table 1: performance indexes are as follows:
as can be seen from the results of the examples and comparative examples in Table 1, the filled polypropylene masterbatch prepared by the present invention has equivalent melt index and deformation temperature under load, but has better rigidity, toughness and strength in tensile strength, elongation at break, flexural strength, flexural modulus and notched izod compared with the polypropylene or polypropylene recycled material. In addition, the regeneration material selected by the invention has wide source and simple production process, thereby greatly saving the cost of raw materials.
These examples are only for illustrating the present invention and should not limit the scope of the present invention. Further, after reading the disclosure of the present invention, one skilled in the art may make various changes or modifications to the equivalent form of the present invention, which also falls within the scope of the claims of the present application.

Claims (6)

1. A polypropylene filling master batch prepared from a polypropylene reclaimed material is characterized in that: the composition is prepared from the following components in parts by weight:
10-20 parts of a polypropylene reclaimed material;
10-30 parts of low-density polyethylene;
2-6 parts of polypropylene grafted acrylic acid;
75-85 parts of inorganic mineral filler;
0.4-1.7 parts of 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane;
0.01-0.02 part of antioxidant;
1.5-3 parts of a lubricant;
the antioxidant is compounded by tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and 6- (4-hydroxy-3, 5-di-tert-butylphenylamino) -2, 4-di-n-octylthio-1, 3, 5-triazine according to the mass ratio of 1: 2;
the preparation method comprises the following steps:
(1) adding the dried polypropylene reclaimed material, low-density polyethylene, polypropylene grafted acrylic acid, an antioxidant and a lubricant into a temperature-controlled high-speed mixer according to the proportion and mixing for 2-3 min; the temperature of the mixer is 75-90 ℃, and the rotating speed is 500-800 r/min;
(2) adding an inorganic mineral filler into the mixture obtained in the step (1) for stirring, adding 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane at a constant speed in the stirring process, and continuously stirring and mixing for 10-15min to obtain a premix;
(3) putting the premix into a double-screw extruder with the length-diameter ratio of 44:1, preheating for 2-4 minutes, and then carrying out melting, extrusion, vacuumizing, air cooling, grain cutting and drying to obtain the polypropylene filling master batch, wherein the temperature of the double-screw extruder is set as follows: the temperature of the pre-melting zone is 140-155 ℃, the temperature of the first melting zone is 190-200 ℃, the temperature of the first high-temperature shearing zone is 200-210 ℃, the temperature of the second high-temperature shearing zone is 210-220 ℃, the temperature of the second melting zone is 200-210 ℃, and the temperature of the discharge hole melting zone is 190-200 ℃; the rotating speed of the double-screw extruder in the processing process is 300-500 rpm.
2. The polypropylene filled masterbatch made of polypropylene reclaimed material according to claim 1, wherein: the recycled polypropylene material is injection molding grade polypropylene which is prepared by sorting, cleaning, crushing and drying after being recycled, the water content of the recycled polypropylene material is lower than 0.5%, the combustion residue is less than 3%, and the melt index is 15-60g/10min under the condition of 2.16kg/230 ℃.
3. The polypropylene filled masterbatch made of polypropylene reclaimed material according to claim 1, wherein: the low density polyethylene has a melt index of 60g/10min at 230 ℃/2.16 Kg.
4. The polypropylene filled masterbatch made of polypropylene reclaimed material according to claim 1, wherein: the grafting rate of the polypropylene grafted acrylic acid is more than or equal to 1.5 percent, and the weight average molecular weight is more than or equal to 20000.
5. The polypropylene filled masterbatch made of polypropylene reclaimed material according to claim 1, wherein: the inorganic mineral filler is one or more of talcum powder, calcium carbonate or mica with the grain diameter of more than or equal to 3000 meshes.
6. The polypropylene filled masterbatch made of polypropylene reclaimed material according to claim 1, wherein: the lubricant is prepared by compounding white mineral oil, ethylene bis stearamide and calcium stearate according to the mass ratio of 2:1: 1.
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