CN111171427A - PE/PP mixed waste plastic high-filling and high-performance composite material and manufacturing method thereof - Google Patents
PE/PP mixed waste plastic high-filling and high-performance composite material and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a PE/PP mixed waste plastic high-filling and high-performance composite material and a manufacturing method thereof, wherein the composite material comprises the following components in parts by weight: 30-70 parts of PE/PP mixed waste plastic, 30-60 parts of filler, 0-11 parts of toughening agent, 0.3-0.4 part of modifier, 0.4-1.2 parts of coupling agent, 0.005-0.01 part of initiator, 0.2-0.4 part of EBS, 0.3-0.5 part of polyethylene wax and 0.2-0.4 part of antioxidant; the modified material can form a composite material with a similar net structure, has the characteristics of high compatibility, high filling, high mechanical property, repeated recycling and the like according to different fillings, and is particularly suitable for products such as blow molding, injection molding, extrusion, calendering and the like.
Description
Technical Field
The invention relates to the field of processing of high polymer materials, in particular to a PE/PP mixed waste plastic high-filling and high-performance composite material and a manufacturing method thereof.
Background
In the field of plastic material modification at present, particularly in the field of waste plastic modification, due to the sorting technology, sorting difficulty is extremely high for different materials with similar polarity, density and application, so that in recycled waste plastic materials, the mixing of different materials is inevitable, and PE and PP belong to the materials.
Since the sources of waste plastics are different, the proportions of the respective mixed materials are also not nearly the same in the sorted mixed waste plastics, and as for the PE and PP materials, both are highly crystalline materials, and when the proportions of the components are not large, both have good compatibility, but when the blending ratio of both is closer to 1: 1, the compatibility of the two is increasingly poor, so that phase separation is generated, and the mechanical property of the mixture is poor; especially when PP is blended in PE, this also brings about differences in processing temperature.
In addition, because the service time of the waste plastics is different and the service environments are different, the material degradation degree of the recycled materials is different, so that the performance difference of the recycled materials is larger, the difficulty of the later-stage recycling modification is increased, and the recycling modification cost is greatly increased. The current situation of modifying recycled plastics is not satisfactory.
Patent application No. CN201710911935.9 "a method for modifying and recycling waste plastics" points out that: the waste plastics include polyethylene terephthalate (PET), High Density Polyethylene (HDPE), Low Density Polyethylene (LDPE), polyvinyl chloride (PVC), polypropylene (PP); the modifier component comprises the following components in percentage by weight: 0-1% of cross-linking agent, 1-5% of light stabilizer, 1-5% of plasticizer, 0.1-0.5% of lubricant and 1-5% of antioxidant.
Patent application No. CN201410430745.1 "a method for modifying and recycling waste plastics" points out that: the modifier comprises 0-1% of cross-linking agent, 1-5% of light stabilizer, 1-5% of plasticizer, 0.1-0.5% of lubricant and 1-5% of antioxidant.
Both of the above patents adopt crosslinking to achieve the purpose of adjusting the basic mechanical properties of the recycled plastic, but have the disadvantages that: the mechanical property is improved by means of crosslinking, and simultaneously, the subsequent recycling is more difficult. The main reason is that the cross-linking forms an unrecoverable network.
Patent No. CN 201811247072.0 "a process for modification treatment of waste plastics" teaches that: the recycled plastic is modified by color mixing, and 30 to 50 percent of TiO2 or CaCO is added3So as to realize the modification of waste plastics and the regeneration of white master batch. This patent only describes simple recycling of recycled plastics and does not achieve high performance, high value added utilization.
What is needed to be solved is the stability, reproducibility and high added value of the modification processing of the recycled plastics.
Disclosure of Invention
The invention aims to solve the technical problem of providing a PE/PP hybrid waste plastic high-filling and high-performance composite material which has high compatibility, high filling and high mechanical property and can be recycled.
In order to solve the technical problems, the technical scheme of the invention is as follows: a PE/PP mixed waste plastic high-filling and high-performance composite material comprises the following components in parts by weight: 30-70 parts of PE/PP mixed waste plastic, 30-60 parts of filler, 0-11 parts of toughening agent, 0.3-0.4 part of modifier, 0.4-1.2 parts of coupling agent, 0.005-0.01 part of initiator, 0.2-0.4 part of ethylene bis stearamide EBS, 0.3-0.5 part of polyethylene wax and 0.2-0.4 part of antioxidant.
As a preferred technical scheme, the filler is one or more of calcium carbonate, talcum powder and silicon micropowder, and the fineness of the filler is 1000-3000 meshes.
As a preferred technical scheme, the toughening agent is a POE, mLLDPE composite toughening agent, wherein the POE: the mass ratio of mLLDPE is 1: 1 or 9: 11 or 11: 9.
as a preferable technical scheme, the synthesis method of the modifier comprises the following steps:
regulating the pH value of formaldehyde to 8-9 by using triethanolamine, and heating to 70-90 ℃;
weighing melamine, wherein the weight of the melamine is 35% -40% of that of the formaldehyde, adding the melamine into the material obtained in the first step, stirring and reacting for 20min, pouring out and condensing the melamine into a solid after the reaction is finished, and drying the condensed solid for later use;
and step three, weighing absolute ethyl alcohol, wherein the weight of the absolute ethyl alcohol is 35% -40% of that of the solid product obtained in the step two, adjusting the absolute ethyl alcohol to a pH value of 3-5.5 by using concentrated hydrochloric acid, concentrated sulfuric acid or concentrated nitric acid, heating to 50-65 ℃, adding the solid prepared in the step two, continuously reacting for 20 minutes, discharging, and solidifying to obtain the modifier.
As a preferred technical scheme, the coupling agent is one or more of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or a silica gel latex emulsion.
As a preferred technical scheme, the initiator is dicumyl peroxide or 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane.
As a preferable technical scheme, the antioxidant is compounded by tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and tri [2, 4-di-tert-butylphenyl ] phosphite in a compounding ratio of 1: 1 or 1: 2.
Due to the adoption of the technical scheme, the PE/PP hybrid waste plastic high-filling and high-performance composite material comprises the following components in parts by weight: 30-70 parts of PE/PP mixed waste plastic, 30-60 parts of filler, 0-11 parts of toughening agent, 0.3-0.4 part of modifier, 0.4-1.2 parts of coupling agent, 0.005-0.01 part of initiator, 0.2-0.4 part of ethylene bis stearamide EBS, 0.3-0.5 part of polyethylene wax and 0.2-0.4 part of antioxidant; the modified material can form a composite material with a similar net structure, has the characteristics of high compatibility, high filling, high mechanical property, repeated recycling and the like according to different fillings, and is particularly suitable for products such as blow molding, injection molding, extrusion, calendering and the like.
The invention aims to solve another technical problem of providing a method for manufacturing a PE/PP mixed waste plastic high-filling high-performance composite material.
In order to solve the technical problems, the technical scheme of the invention is as follows: a method for manufacturing a PE/PP mixed waste plastic high-filling high-performance composite material comprises the following manufacturing steps:
pouring 30-60 parts by weight of filler into a high-speed mixer, starting high-speed stirring to 100 ℃, continuing to dry for 20min, adding 0.4-1.2 parts by weight of coupling agent, continuing to stir for 5min, and discharging to prepare active filler;
weighing the weight of the modifier and the initiator required by the formula, weighing the active filler obtained in the step one according to ten times of the total weight of the modifier and the initiator, pouring the active filler into a small high-speed mixer together, stirring and mixing for 5min, and discharging to obtain a modifier and an initiator amplified material;
weighing the PE/PP mixed material, the toughening agent, the ethylene bis stearamide EBS, the polyethylene wax and the antioxidant according to the proportion;
step four, putting the materials weighed in the step three and the rest active filler in the step two into a low-speed mixer together, mixing for 5min, and putting into a storage bin;
setting the temperature of a granulator to be 140-210 ℃, the temperature of a water tank to be 55-68 ℃, adjusting the rotating speed of a main machine to be 420-450 rad/min and the feeding rotating speed to be 28-35 rad/min, and controlling the front end to be vacuumized at 0.6-0.8 MPa and the rear end to be vacuumized at not less than 1.2 MPa;
and step six, adjusting the rotation speed of the underwater granulator to match with the extrusion speed, sequentially passing through a dehydration bin, a vibrating screen, a fan, a middle bin and a homogenization bin, and finally packaging into a finished product.
As a preferred technical scheme, the granulator adopts a double-screw granulator, and the L/D is 44/1.
As a preferred technical scheme, the granulator is connected with a double-vacuum devolatilization device, wherein a scroll vacuum pump is adopted for front devolatilization, and a screw vacuum pump is adopted for rear devolatilization.
According to the technical scheme, the PE/PP hybrid waste plastic high-filling and high-performance composite material is manufactured by utilizing the characteristics that the PE and PP materials are subjected to chain scission under the action of an initiator at high temperature to generate free radicals, and simultaneously, the generated free radicals have high activity and are easy to initiate chain scission degradation or crosslinking.
Detailed Description
The invention is further illustrated by the following examples. In the following detailed description, certain exemplary embodiments of the present invention are described by way of illustration only. Needless to say, a person skilled in the art realizes that the described embodiments can be modified in various different ways without departing from the spirit and scope of the present invention.
A PE/PP mixed waste plastic high-filling and high-performance composite material comprises the following components in parts by weight: 30-70 parts of PE/PP mixed waste plastic, 30-60 parts of filler, 0-11 parts of toughening agent, 0.3-0.4 part of modifier, 0.4-1.2 parts of coupling agent, 0.005-0.01 part of initiator, 0.2-0.4 part of ethylene bis stearamide EBS, 0.3-0.5 part of polyethylene wax and 0.2-0.4 part of antioxidant.
The PE/PP mixed waste plastic is any PE and PP mixed waste plastic which is recycled and granulated in the recycling market. The filler is one or more of calcium carbonate, talcum powder and silica powder, calcium carbonate is preferred, and the fineness of the filler is 1000-3000 meshes. The toughening agent is a POE and mLLDPE composite toughening agent, wherein the POE: the mass ratio of mLLDPE is 1: 1 or 9: 11 or 11: 9.
the synthesis method of the modifier comprises the following steps:
regulating the pH value of formaldehyde to 8-9 by using triethanolamine, and heating to 70-90 ℃;
weighing melamine, wherein the weight of the melamine is 35% -40% of that of the formaldehyde, adding the melamine into the material obtained in the first step, stirring and reacting for 20min, pouring out and condensing the melamine into a solid after the reaction is finished, and drying the condensed solid for later use;
and step three, weighing absolute ethyl alcohol, wherein the weight of the absolute ethyl alcohol is 35% -40% of that of the solid product obtained in the step two, adjusting the absolute ethyl alcohol to a pH value of 3-5.5 by using concentrated hydrochloric acid, concentrated sulfuric acid or concentrated nitric acid, heating to 50-65 ℃, adding the solid prepared in the step two, continuously reacting for 20 minutes, discharging, and solidifying to obtain the modifier.
The synthesized modifier has 3-4 active groups, the active groups are broken at the temperature of 120-145 ℃ to form active free radicals, the function of breakpoint splicing is achieved, and the composite effects of improving the mechanical property and compatibility of materials and the like are achieved when the modifier is applied to polymers.
the initiator is dicumyl peroxide or 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, the antioxidant is compounded by pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and tris [2, 4-di-tert-butylphenyl ] phosphite in a compounding ratio of 1: 1 or 1: 2.
The modified material can form a composite material with a similar net structure, has the characteristics of high compatibility, high filling, high mechanical property, repeated recycling and the like according to different fillings, and is particularly suitable for products such as blow molding, injection molding, extrusion, calendering and the like.
A method for manufacturing a PE/PP mixed waste plastic high-filling high-performance composite material comprises the following manufacturing steps:
pouring 30-60 parts by weight of filler into a high-speed mixer, starting high-speed stirring to 100 ℃, continuing to dry for 20min, adding 0.4-1.2 parts by weight of coupling agent, continuing to stir for 5min, and discharging to prepare active filler;
weighing the weight of the modifier and the initiator required by the formula, weighing the active filler obtained in the step one according to ten times of the total weight of the modifier and the initiator, pouring the active filler into a small high-speed mixer together, stirring and mixing for 5min, and discharging to obtain a modifier and an initiator amplified material;
weighing the PE/PP mixed material, the toughening agent, the ethylene bis stearamide EBS, the polyethylene wax and the antioxidant according to the proportion;
step four, putting the materials weighed in the step three and the rest active filler in the step two into a low-speed mixer together, mixing for 5min, and putting into a storage bin;
setting the temperature of a granulator to be 140-210 ℃, the temperature of a water tank to be 55-68 ℃, adjusting the rotating speed of a main machine to be 420-450 rad/min and the feeding rotating speed to be 28-35 rad/min, and controlling the front end to be vacuumized at 0.6-0.8 MPa and the rear end to be vacuumized at not less than 1.2 MPa;
and step six, adjusting the rotation speed of the underwater granulator to match with the extrusion speed, sequentially passing through a dehydration bin, a vibrating screen, a fan, a middle bin and a homogenization bin, and finally packaging into a finished product.
In the fifth step, the granulator is a double-screw granulator, and the L/D is 44/1.
In the sixth step, the granulator is connected with a double vacuum devolatilization device, wherein a scroll vacuum pump is adopted for front devolatilization, and a screw vacuum pump is adopted for rear devolatilization.
The manufacturing method utilizes the characteristics that PE and PP materials are subjected to chain scission under the action of an initiator at high temperature to generate free radicals, and the generated free radicals have high activity and are easy to initiate chain scission degradation or crosslinking.
By adopting different proportions, PE/PP hybrid composite materials with different performance indexes can be produced, and the recovered plastics with fixed PE/PP hybrid proportion are exemplified below.
the proportion of PE in the PE/PP mixed waste plastic is about 80 percent, the toughening agent is compounded by POE and mLLDPE in a ratio of 1.1: 0.9, the coupling agent is silica gel latex emulsion, the filler is 3000-mesh calcium carbonate, the initiator is 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, and the antioxidant is compounded by tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and tri [ 2.4-di-tert-butylphenyl ] phosphite in a ratio of 1: 2.
Step one, pouring 3000-mesh calcium carbonate into a high-speed mixer, starting high-speed stirring to 100 ℃, continuing to dry for 20min, adding the weighed coupling agent, continuing to stir for 5min, and discharging to obtain the active calcium carbonate.
Step two, weighing the modifier and the initiator required by the formula, weighing the active calcium carbonate obtained in the step one according to 10 times of the total amount of the modifier and the initiator, pouring the active calcium carbonate into a small-sized high-speed mixer, stirring and mixing for 5min, and discharging to obtain a modifier and an initiator amplification material;
weighing the PE/PP mixed material, the toughening agent, the ethylene bis stearamide EBS, the polyethylene wax and the antioxidant;
step four, putting all the materials weighed in the step three and the residual calcium carbonate in the step two into a low-speed mixer together, mixing for 5min, and putting into a bin;
step five, setting the temperature of the granulator to 160 ℃, 180 ℃, 195 ℃, 210 ℃, 200 ℃, 185 ℃, 170 ℃, 145 ℃, 160 ℃, 185 ℃, 180 ℃ and 65 ℃ of the water tank. Adjusting the rotating speed of the main machine to 420rad/min and the feeding rotating speed to 31 rad/min; controlling the front end to be vacuumized by 0.6-0.8 MPa, and controlling the rear end to be vacuumized by not less than 1.2 MPa.
And step six, adjusting the rotation speed of the underwater granulator to be matched with the extrusion speed, and packaging the underwater granulator into a finished product through dehydration, a vibrating screen, a fan, a middle bin and a homogenizing bin, wherein the moisture content of the finished product is controlled to be less than or equal to 0.15%.
Table 1 comparative and example formulation tables:
the test properties of the materials produced according to the comparative and exemplary formulation tables of table 1 are shown in table 2.
TABLE 2 Performance Table for materials of the test formulation
Of course, the PE/PP mixed waste plastic high-filling and high-performance composite material and the manufacturing method thereof can also be used for producing single PE reclaimed materials or PP reclaimed materials, and similar formula structures can also be used for producing materials such as PA, PBT and the like. Can produce high-performance, high-filling and recyclable modified materials, and is an effective way for improving the high performance of the recycled plastics.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A PE/PP mixed waste plastic high-filling and high-performance composite material is characterized by comprising the following components in parts by weight: 30-70 parts of PE/PP mixed waste plastic, 30-60 parts of filler, 0-11 parts of toughening agent, 0.3-0.4 part of modifier, 0.4-1.2 parts of coupling agent, 0.005-0.01 part of initiator, 0.2-0.4 part of ethylene bis stearamide EBS, 0.3-0.5 part of polyethylene wax and 0.2-0.4 part of antioxidant.
2. The PE/PP hybrid waste plastic highly-filled and highly-functionalized composite material as claimed in claim 1, wherein the filler is one or more of calcium carbonate, talcum powder and silica powder, and the fineness of the filler is 1000-3000 meshes.
3. The PE/PP hybrid waste plastic highly filled and high performance composite material as claimed in claim 1, wherein the toughening agent is a POE, mLLDPE composite toughening agent, wherein the ratio of POE: the mass ratio of mLLDPE is 1: 1 or 9: 11 or 11: 9.
4. the PE/PP hybrid waste plastic highly-filled and highly-functionalized composite material according to claim 1, wherein the modifier is synthesized by the following method:
regulating the pH value of formaldehyde to 8-9 by using triethanolamine, and heating to 70-90 ℃;
weighing melamine, wherein the weight of the melamine is 35% -40% of that of the formaldehyde, adding the melamine into the material obtained in the first step, stirring and reacting for 20min, pouring out and condensing the melamine into a solid after the reaction is finished, and drying the condensed solid for later use;
and step three, weighing absolute ethyl alcohol, wherein the weight of the absolute ethyl alcohol is 35% -40% of that of the solid product obtained in the step two, adjusting the absolute ethyl alcohol to a pH value of 3-5.5 by using concentrated hydrochloric acid, concentrated sulfuric acid or concentrated nitric acid, heating to 50-65 ℃, adding the solid prepared in the step two, continuously reacting for 20 minutes, discharging, and solidifying to obtain the modifier.
5. The PE/PP hybrid waste plastic highly-filled and high-performance composite material as claimed in claim 1, wherein the coupling agent is one or more of a silane coupling agent, a titanate coupling agent, an aluminate coupling agent or a silica gel latex emulsion.
6. The PE/PP hybrid waste plastic highly filled, high performing composite material according to claim 1, wherein the initiator is dicumyl peroxide or 2, 5-dimethyl-2, 5-di (t-butylperoxy) hexane.
7. the PE/PP hybrid waste plastic highly-filled and highly-functionalized composite material as claimed in claim 1, wherein the antioxidant is a mixture of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and tris [2, 4-di-tert-butylphenyl ] phosphite in a ratio of 1: 1 or 1: 2.
8. The method for producing a highly filled and high performance composite material of PE/PP hybrid waste plastic according to claim 1, comprising the steps of:
pouring 30-60 parts by weight of filler into a high-speed mixer, starting high-speed stirring to 100 ℃, continuing to dry for 20min, adding 0.4-1.2 parts by weight of coupling agent, continuing to stir for 5min, and discharging to prepare active filler;
weighing the weight of the modifier and the initiator required by the formula, weighing the active filler obtained in the step one according to ten times of the total weight of the modifier and the initiator, pouring the active filler into a small high-speed mixer together, stirring and mixing for 5min, and discharging to obtain a modifier and an initiator amplified material;
weighing the PE/PP mixed material, the toughening agent, the ethylene bis stearamide EBS, the polyethylene wax and the antioxidant according to the proportion;
step four, putting the materials weighed in the step three and the rest active filler in the step two into a low-speed mixer together, mixing for 5min, and putting into a storage bin;
setting the temperature of a granulator to be 140-210 ℃, the temperature of a water tank to be 55-68 ℃, adjusting the rotating speed of a main machine to be 420-450 rad/min and the feeding rotating speed to be 28-35 rad/min, and controlling the front end to be vacuumized at 0.6-0.8 MPa and the rear end to be vacuumized at not less than 1.2 MPa;
and step six, adjusting the rotation speed of the underwater granulator to match with the extrusion speed, sequentially passing through a dehydration bin, a vibrating screen, a fan, a middle bin and a homogenization bin, and finally packaging into a finished product.
9. The method for producing a PE/PP hybrid waste plastic highly-filled and high-performance composite material as claimed in claim 8, wherein the pelletizer is a twin-screw pelletizer, and L/D is 44/1.
10. The method for manufacturing a PE/PP hybrid waste plastic highly-filled and highly-functional composite material as claimed in claim 8, wherein the pelletizer is connected with a double vacuum devolatilization apparatus, wherein a scroll vacuum pump is used for the front devolatilization, and a screw vacuum pump is used for the rear devolatilization.
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| CN113388192A (en) * | 2021-04-20 | 2021-09-14 | 长泰铱科科技有限公司 | High-toughness low-temperature-resistant highlight regenerated PP (polypropylene) modified material and preparation method thereof |
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