CN110643116A - High-strength polyolefin composite material for packaging bag and preparation method thereof - Google Patents
High-strength polyolefin composite material for packaging bag and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength polyolefin composite material for packaging bags and a preparation method thereof, wherein the high-strength polyolefin composite material comprises the following raw materials in parts by weight: 60-80 parts of polyolefin matrix, 10-15 parts of functionalized graphene, 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant. According to the invention, the polyolefin matrix and the functionalized graphene are mixed, then the glass fiber, the coupling agent and the antioxidant are added, and the high-strength polyolefin composite material containing graphene for the packaging bag is prepared in a microwave heating reactor in a microwave heating mode, the compatibility of the graphene and the polyolefin is improved through the functionalized graphene, and the mechanical properties of the bending strength, the notch impact strength, the tensile strength and the breaking strength of the polyolefin composite material are improved; the preparation method provided by the invention has the advantages of small graphene consumption, simple preparation method, low cost and easiness in implementation.
Description
Technical Field
The invention belongs to the technical field of polyolefin composite materials, and particularly relates to a high-strength polyolefin composite material for a packaging bag and a preparation method thereof.
Background
The polyolefin composite material is widely applied to industries such as automobiles, household appliances, packaging and the like. The modified and processed polyolefin composite material can meet the normal use requirement in the use performance of all aspects. However, polyolefin composites release volatile substances containing some bad smells or harmful to human health to various degrees during high-temperature processing and use, and this problem has attracted the attention of governments, various mass production enterprises at home and abroad, and resin manufacturers. Therefore, the technical development of the low-odor polyolefin composite material has the realistic significance of environmental protection.
The graphene nanocomposite is prepared by uniformly dispersing graphene in a polymer matrix material by using a polymer matrix as a continuous phase and graphene as a dispersed phase through a proper preparation method to form a composite system containing a nano-sized material. The graphene nanocomposite not only has the surface effect and the quantum size effect of the nanomaterial, but also combines the rigidity, the dimensional stability and the thermal stability of the nanofiller with the toughness, the processability and the dielectric property of the polymer, thereby generating a plurality of excellent properties. The main polymer matrix of the graphene nanocomposite material comprises: nylon-6, polycarbonate, epoxy resin, polyurethane, polystyrene, polymethyl methacrylate, styrene-isoprene-styrene block copolymer, and the like. And few research reports on graphene/polyolefin composite materials are reported.
The invention patent with the publication number of CN104926960A discloses a method for preparing a diolefin polymerization catalyst with graphene/magnesium chloride as a carrier by an in-situ polymerization process. The invention patent with publication number CN105504469A discloses a method for preparing a graphene/polyolefin elastomer master batch and a graphene antistatic composite material by a solution compounding process. However, both the in-situ polymerization process and the solution compounding process have the disadvantages of high discharge, low efficiency and difficult scale-up.
The invention patent with the publication number of CN104098816A provides a polyolefin/graphene nanocomposite and a preparation method thereof, wherein the method for functionally modifying graphene in the method has the advantages of relatively more preparation procedures, low modification efficiency and relatively higher cost; the patent of the invention with the publication number of CN105570560A mentions a graphene-enhanced thermal conductivity composite polyolefin pipe, and the patent of the invention with the publication number of CN103739929A proposes a graphene-containing polyolefin high-semiconductive shielding material for cables and a preparation method thereof, wherein the two patents adopt a melting composite process, but the prepared composite material has poor dispersion effect, and the industrial preparation and application of the polyolefin-based graphene composite material are not easy to directly realize.
Polypropylene materials have high rigidity but low impact strength, especially low temperature impact strength; the high-density polyethylene material has good chemical stability and toughness, but has poor rigidity, low heat-resistant temperature, low surface smoothness, easy deformation, easy stress cracking and low surface hardness compared with polypropylene. It is therefore often necessary to modify both materials to achieve a particular application.
Polyolefin compositions containing polyethylene, polypropylene and rubber have been receiving wide attention, and optimization of properties such as rigidity and toughness can be achieved by matching of various components, thereby meeting the needs of specific products. Such compositions are currently used in a variety of applications such as automotive, packaging and ware.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a high-strength polyolefin composite material for a packaging bag and a preparation method thereof, wherein the high-strength polyolefin composite material is reinforced by graphene, and is hopefully reinforced and has excellent polyolefin composite material; the preparation method can effectively reduce the odor of the polyolefin composite material obtained by production, does not change the original performance of the polyolefin composite material, and is simple, low in production cost and convenient for industrial application.
The technique and method adopted by the present invention to solve the above problems are as follows:
a high-strength polyolefin composite material for packaging bags comprises the following raw materials in parts by weight: 60-80 parts of polyolefin matrix, 10-15 parts of functionalized graphene, 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant.
Further, the polyolefin matrix is selected from one or two of random copolymerized polypropylene (PPR) and high-density polyethylene.
Further, the polyolefin elastomer is ethylene-octene copolymer (POE).
Further, the coupling agent is selected from one of a chromium complex coupling agent, a silane coupling agent, a titanate coupling agent or other coupling agents.
Further, the antioxidant is selected from one or more of pentaerythritol tetrakis (beta- (3,5(3,5(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) (1010), bis (2,4(2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphite (626), and dilauryl thiodipropionate (DLTP).
Further, the functionalized graphene is obtained by a reduction method of modified graphene oxide, and the reduction method of the modified graphene oxide is as follows: dispersing freeze-dried modified graphene oxide in organic phases of dimethylbenzene and normal hexane, adding oxalic acid and a sodium borohydride reducing agent to obtain graphene with a certain reduction degree, and then freezing and drying the graphene;
wherein the addition amount of the reducing agent is 0.1-2.0 times of the mass of the modified graphene oxide.
Further, the preparation method of the high-strength polyolefin composite material for the packaging bag comprises the following specific steps:
s1, premixing 60-80 parts of polyolefin matrix and 10-15 parts of functionalized graphene at high speed to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 160-280 ℃, and the reaction time is 3-600S, and the microwave heating conditions are as follows: the microwave power is 50-8000W, and the microwave frequency is 500-270000 MHz; obtaining a prefabricated material;
and S4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag.
Further, the microwave heating temperature in the step S3 is 160-260 ℃, and the reaction lasts 10-400S.
Further, the conditions of the microwave heating in the step S3 are as follows: the microwave power is 300-6000W, and the microwave frequency is 700-240000 MHz.
Further, the heating temperature in the step S4 is 220-.
According to the invention, the polyolefin matrix and the functionalized graphene are mixed, then the glass fiber, the coupling agent and the antioxidant are added, a microwave heating mode is adopted, and the microwave power, the microwave frequency, the microwave heating temperature and the microwave heating time are reasonably regulated, so that heat can permeate into polyolefin macromolecules, unnecessary over-reaction caused by local overheating is avoided, the amount of polyolefin or additive decomposed into odorous micromolecular compounds during the production of polyolefin composite materials is effectively reduced, and the odor of the polyolefin composite materials is obviously reduced; the high-strength polyolefin composite material containing graphene for the packaging bag is prepared, the compatibility of the graphene and the polyolefin is improved through the functionalized graphene, and the mechanical properties of the bending strength, the notch impact strength, the tensile strength and the breaking strength of the polyolefin composite material are improved; the polyolefin composite material has excellent performances such as wear resistance, bending, notch impact, fracture, thermal stability and the like, opens up a new application field containing the nano graphene material, and can be applied to various fields such as packaging materials and the like; the preparation method disclosed by the invention is less in graphene consumption, simple in preparation method, low in cost, green and environment-friendly, and easy to implement, and cannot influence the performance of the polyolefin composite material.
The graphene is used for reinforcing the polyolefin material to obtain a reinforced polyolefin composite material with excellent wear-resisting property; the material has very high normal-temperature and low-temperature notch impact strength, especially low-temperature notch impact strength, and excellent rigidity-toughness balance performance;
the glass fiber is added and selected as a reinforcing material, so that the comprehensive mechanical property of the material can be effectively improved, and the cost is reduced, the type of the glass fiber is not particularly limited, and the glass fiber can be glass fiber in polyolefin composite materials commonly used in the field, preferably, the fiber diameter of the glass fiber is 10-14 μm, and the linear density is 800-.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention and to thereby define the scope of the invention more clearly;
the technical scheme of the invention is that the high-strength polyolefin composite material for the packaging bag comprises the following raw materials in parts by weight: 60-80 parts of polyolefin matrix, 10-15 parts of functionalized graphene, 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant.
The polyolefin matrix is selected from one or two of random copolymerization polypropylene (PPR) and high density polyethylene.
The polyolefin elastomer is ethylene-octene copolymer (POE).
The coupling agent is selected from one of a chromium complex coupling agent, a silane coupling agent, a titanate coupling agent or other coupling agents.
The antioxidant is selected from one or more of pentaerythritol tetrakis (beta- (3,5(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) (1010), bis (2,4(2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphite (626), and dilauryl thiodipropionate (DLTP).
The functionalized graphene is obtained by a reduction method of modified graphene oxide, and the reduction method of the modified graphene oxide comprises the following steps: dispersing freeze-dried modified graphene oxide in organic phases of dimethylbenzene and normal hexane, adding oxalic acid and a sodium borohydride reducing agent to obtain graphene with a certain reduction degree, and then freezing and drying the graphene;
wherein the addition amount of the reducing agent is 0.1-2.0 times of the mass of the modified graphene oxide.
Example 1
The embodiment of the invention provides a preparation method of a high-strength polyolefin composite material for packaging bags, which comprises the following specific steps:
s1, performing high-speed premixing on 60 parts of random copolymerization polypropylene (PPR) selected as a polyolefin matrix and 10 parts of functionalized graphene to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 10 parts of polyolefin elastomer, 3 parts of glass fiber, 1 part of coupling agent and 0.5 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 200 ℃, the reaction time is 200S, and the microwave heating conditions are as follows: the microwave power is 1000W, and the microwave frequency is 250000 MHz; obtaining a prefabricated material;
s4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag, wherein the heating temperature is 220 ℃.
Example 2
The embodiment of the invention provides a preparation method of a high-strength polyolefin composite material for packaging bags, which comprises the following specific steps:
s1, selecting 70 parts of high-density polyethylene as a polyolefin matrix and 12 parts of functionalized graphene, and carrying out high-speed premixing to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 15 parts of polyolefin elastomer, 5 parts of glass fiber, 2 parts of coupling agent and 0.8 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 250 ℃, the reaction time is 400S, and the microwave heating conditions are as follows: the microwave power is 3000W, and the microwave frequency is 50000 MHz; obtaining a prefabricated material;
s4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag, wherein the heating temperature is 230.
Example 3
The embodiment of the invention provides a preparation method of a high-strength polyolefin composite material for packaging bags, which comprises the following specific steps:
s1, selecting 80 parts of random copolymerization polypropylene (PPR) and High Density Polyethylene (HDPE) as polyolefin matrixes, and premixing with 15 parts of functionalized graphene at high speed to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 20 parts of polyolefin elastomer, 6 parts of glass fiber, 3 parts of coupling agent and 1 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 230 ℃, and the reaction time is 80S, and the microwave heating conditions are as follows: the microwave power is 6000W, and the microwave frequency is 800 MHz; obtaining a prefabricated material;
s4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag, wherein the heating temperature is 240 ℃.
Example 4
The embodiment of the invention provides a preparation method of a high-strength polyolefin composite material for packaging bags, which comprises the following specific steps:
s1, selecting 80 parts of high-density polyethylene as a polyolefin matrix and 10 parts of functionalized graphene, and carrying out high-speed premixing to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 20 parts of polyolefin elastomer, 3 parts of glass fiber, 1 part of coupling agent and 0.5 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 160 ℃, and the reaction time is 10S, and the microwave heating conditions are as follows: the microwave power is 4500W, and the microwave frequency is 2000 MHz; and obtaining a prefabricated material.
S4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag, wherein the heating temperature is 220 ℃.
Example 5
The embodiment of the invention provides a preparation method of a high-strength polyolefin composite material for packaging bags, which comprises the following specific steps:
s1, premixing 60 parts of polyolefin matrix and 15 parts of functionalized graphene at high speed to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 10 parts of polyolefin elastomer, 6 parts of glass fiber, 3 parts of coupling agent and 1 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 250 ℃, the reaction time is 80S, and the microwave heating conditions are as follows: the microwave power is 2000W, and the microwave frequency is 200000 MHz; obtaining a prefabricated material;
s4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag, wherein the heating temperature is 240 ℃.
Comparative example 1
The coupling agent in example 1 was changed to a common coupling agent without using an antioxidant, and the microwave heating reactor in step S3 was changed to a conventional reaction tank (electric heating), and the other raw materials and the preparation method were not changed.
Comparative example 2
The functionalized graphene in example 2 was changed to unmodified graphene oxide without using an antioxidant, and the microwave heating reactor in step S3 was changed to a conventional reaction tank (electrical heating), and the other raw materials and preparation method were not changed.
Comparative example 3
The functionalized graphene in example 3 was changed to unmodified graphene oxide, no coupling agent was used, the microwave heating reactor in step S3 was changed to a conventional reaction tank (electrical heating), and the other raw materials and preparation method were not changed.
Comparative example 4
The microwave heating reactor in step S3 was changed to a conventional reaction tank (electric heating) without using functionalized graphene in example 4, and other raw materials and preparation methods were not changed.
Comparative example 5
The microwave heating reactor in step S3 was changed to a conventional reaction tank (electric heating) without using glass fiber in example 5, and other raw materials and preparation methods were not changed.
Test example
The polyolefin composites prepared in examples 1 to 5 and comparative examples 1 to 5 were subjected to the performance test, and the results are shown in the table. The following methods were referenced, respectively: according to the JB/T9226-2008 standard, the test of mechanical property (GB1040-79) and thermal stability (GB/T14837-:
TABLE 1 polyolefin composites prepared in examples 1-5 and comparative examples 1-5 Performance parameters
The polyolefin composites obtained in examples 1 to 5 of the present invention and comparative examples 1 to 5 were subjected to odor evaluation using the following criteria:
placing the polyolefin composite material into a special odor bottle, sealing the odor bottle, and placing the odor bottle into a blast oven at 80 ℃ for constant-temperature storage for 2 hours; the odor bottle was then removed and allowed to cool to 30 ℃ at room temperature, and the odor assessor quickly removed the cap of the odor bottle (which cap could not be lifted) and performed an odor assessment; each sample required 5 odor evaluators for odor evaluation according to the odor rating scale of table 1.
Table 2 odor test evaluation scale
When the maximum minus the minimum of the 5 odor assessor ratings is less than 1.5, then the odor progression is the average of the 5 odor assessor ratings. The average number of stages can be about 0.5, and the specific rule is as follows: when the value after the decimal point of the average series is less than 0.25, the value after the decimal point is cut off (for example, 3.22 is taken as 3.0); when the value after the decimal point of the average number is greater than or equal to 0.25 and less than 0.75, the value after the decimal point is about to 0.5 (for example, 3.33 or 3.73 takes 3.5); when the value after the average stage decimal point is greater than or equal to 0.75, the numerical value is advanced by one bit (for example, 3.77 is 4.0); when the minimum value subtracted from the maximum value in the rating of 5 odor evaluators is 1.5, the average value of the remaining three values is calculated after the maximum value and the minimum value are removed; when the maximum minus the minimum of the 5 odor assessors ratings is greater than 1.5, the odor rating needs to be reevaluated.
The experimental effects are shown in table 3;
table 3 shows the odor rating data of the polyolefin composites obtained in examples 1 to 5 of the present invention and comparative examples 1 to 5
| Example of the implementation | Microwave power/W | Microwave frequency/MHz | Temperature/. degree.C | time/S | Smell/grade |
| Example 1 | 1000 | 250000 | 200 | 200 | 3.0 |
| Example 2 | 3000 | 50000 | 250 | 400 | 2.6 |
| Example 3 | 6000 | 800 | 230 | 80 | 2.7 |
| Example 4 | 4500 | 2000 | 160 | 10 | 2.9 |
| Example 5 | 2000 | 200000 | 200 | 200 | 2.8 |
| Comparative example 1 | 200 | 200 | 4.1 | ||
| Comparative example 2 | 250 | 400 | 3.9 | ||
| Comparative example 3 | 230 | 80 | 3.8 | ||
| Comparative example 4 | 160 | 10 | 4.5 | ||
| Comparative example 5 | 200 | 200 | 4.2 |
The above description is only for the specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any changes or substitutions that are not thought of by the inventive labor should be covered within the protection scope of the present invention, and therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.
Claims (10)
1. The high-strength polyolefin composite material for the packaging bag is characterized by comprising the following raw materials in parts by weight: 60-80 parts of polyolefin matrix, 10-15 parts of functionalized graphene, 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant.
2. The high-strength polyolefin composite material for packaging bags according to claim 1, wherein: the polyolefin matrix is selected from one or two of random copolymerization polypropylene (PPR) and high density polyethylene.
3. The high-strength polyolefin composite material for packaging bags according to claim 1, wherein: the polyolefin elastomer is ethylene-octene copolymer (POE).
4. The high-strength polyolefin composite material for packaging bags according to claim 1, wherein: the coupling agent is selected from one of a chromium complex coupling agent, a silane coupling agent, a titanate coupling agent or other coupling agents.
5. The high-strength polyolefin composite material for packaging bags according to claim 1, wherein: the antioxidant is selected from one or more of pentaerythritol tetrakis (beta- (3,5(3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) (1010), bis (2,4(2, 4-di-tert-butyl-phenyl) pentaerythritol diphosphite (626), and dilauryl thiodipropionate (DLTP).
6. The high-strength polyolefin composite material for packaging bags according to claim 1, wherein: the functionalized graphene is obtained by a reduction method of modified graphene oxide, and the reduction method of the modified graphene oxide comprises the following steps: dispersing freeze-dried modified graphene oxide in organic phases of dimethylbenzene and normal hexane, adding oxalic acid and a sodium borohydride reducing agent to obtain graphene with a certain reduction degree, and then freezing and drying the graphene;
wherein the addition amount of the reducing agent is 0.1-2.0 times of the mass of the modified graphene oxide.
7. The method for preparing a high-strength polyolefin composite material for a packaging bag according to claim 1, wherein: the method comprises the following specific steps:
s1, premixing 60-80 parts of polyolefin matrix and 10-15 parts of functionalized graphene at high speed to obtain a premixed material;
s2, blending the premixed material obtained in the step S1 with 10-20 parts of polyolefin elastomer, 3-6 parts of glass fiber, 1-3 parts of coupling agent and 0.5-1 part of antioxidant to obtain a mixed material;
s3, placing the mixed material obtained in the step S2 into a microwave heating reactor, wherein the microwave heating temperature is 160-280 ℃, and the reaction time is 3-600S, and the microwave heating conditions are as follows: the microwave power is 50-8000W, and the microwave frequency is 500-270000 MHz; obtaining a prefabricated material;
and S4, adding the prefabricated material into a film blowing machine, heating, blowing out, cooling and pressing edges to obtain the high-strength polyolefin composite material for the packaging bag.
8. The method for preparing a high-strength polyolefin composite material for a packaging bag according to claim 7, wherein: the microwave heating temperature in the step S3 is 160-260 ℃, and the reaction lasts 10-400S.
9. The method for preparing a high-strength polyolefin composite material for a packaging bag according to claim 7, wherein: the microwave heating conditions in step S3 are as follows: the microwave power is 300-6000W, and the microwave frequency is 700-240000 MHz.
10. The method for preparing a high-strength polyolefin composite material for a packaging bag according to claim 7, wherein: the heating temperature in step S4 is 220-240.
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