CN115838530B - Modified PET composite material and preparation method thereof - Google Patents
Modified PET composite material and preparation method thereof Download PDFInfo
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- CN115838530B CN115838530B CN202310114873.4A CN202310114873A CN115838530B CN 115838530 B CN115838530 B CN 115838530B CN 202310114873 A CN202310114873 A CN 202310114873A CN 115838530 B CN115838530 B CN 115838530B
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Abstract
The invention relates to the technical field of high polymer materials, and provides a modified PET composite material and a preparation method thereof, wherein the modified PET composite material comprises the following components in parts by weight: 60-70 parts of PET, 30-40 parts of PC, 8-12 parts of trimethylolpropane triglycidyl ether, 0.5-1 part of antioxidant, 4-8 parts of modified clay and 1-2 parts of lubricant; the preparation method of the modified PET composite material comprises the following steps: mixing PET, PC, trimethylolpropane triglycidyl ether, an antioxidant, modified clay and a lubricant, and extruding the mixture through an extruder to obtain the modified PET composite material. Through the technical scheme, the problems of high brittleness and poor toughness of PET materials in the prior art are solved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a modified PET composite material and a preparation method thereof.
Background
Polyethylene terephthalate (PET) has a series of excellent characteristics of light density, high strength, high rigidity, good heat resistance, chemical resistance, low price and the like, and can be recycled, so that the PET has wide application in national economy, national defense industry and high and new technology industry, and is an indispensable novel material. However, brittle fracture due to notch sensitivity is one of the reasons that limits its application as an engineering structural material, and modification of PET materials is therefore required.
Disclosure of Invention
The invention provides a modified PET composite material and a preparation method thereof, which solve the problems of high brittleness and poor toughness of PET materials in the related art.
The technical scheme of the invention is as follows:
the modified PET composite material comprises the following components in parts by weight: 60-70 parts of PET, 30-40 parts of PC, 8-12 parts of trimethylolpropane triglycidyl ether, 0.5-1 part of antioxidant, 4-8 parts of modified clay and 1-2 parts of lubricant.
The antioxidant comprises one or more of antioxidant 1010, antioxidant TNP and antioxidant TPP.
The lubricant comprises one or more of pentaerythritol stearate and ethylene bis-stearamide.
The modified clay is obtained by treating clay with p-ethoxyformylphenyl propionaldehyde and isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate.
The preparation method of the modified clay comprises the following steps:
a1, mixing clay and water to obtain a mixture I;
a2, adding p-ethoxyformylphenyl propionaldehyde and isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the mixture I, heating to 80-100 ℃, and treating for 2-3h to obtain a mixture II;
and A3, filtering, washing and drying the mixture II to obtain the modified clay.
The clay content of the mixture I in the A1 is 20-25%.
The adding amount of the p-ethoxyformylbenzene propionaldehyde in the A2 is 1-2% of the mass of the mixture I, and the adding amount of the isopropyl tri (dioctyl pyrophosphoryloxy) titanate in the A2 is 2-4% of the mass of the mixture I.
The mass ratio of the p-ethoxyformylphenyl propionaldehyde to the isopropyl tri (dioctyl pyrophosphoryl oxy) titanate in the A2 is 1:2.
The preparation method of the modified PET composite material comprises the following steps: mixing PET, PC, trimethylolpropane triglycidyl ether, an antioxidant, modified clay and a lubricant, and extruding the mixture through an extruder to obtain the modified PET composite material.
The extruder is a double-screw extruder, and the technological parameters of the double-screw extruder are as follows: the temperature of the first area is 190-200 ℃; the temperature of the second area is 210-220 ℃; the temperature of the third region is 230-250 ℃; the temperature of the fourth area is 255-265 ℃; the temperature of the fifth area is 265-275 ℃; the temperature of the six areas is 255-265 ℃; the temperature of the seventh area is 250-260 ℃; the temperature of the eighth zone is 240-250 ℃; the temperature of the machine head is 255-270 ℃, and the rotating speed of the screw is 250-350rpm.
The working principle and the beneficial effects of the invention are as follows:
1. according to the invention, the trimethylolpropane triglycidyl ether is adopted to blend with PET and PC to prepare the composite material, and the addition of the trimethylolpropane triglycidyl ether enables the PET and PC to be crosslinked on one hand, so that the tensile strength and impact strength of the PET composite material are improved, the brittleness of the composite material is reduced, and on the other hand, the introduction of the trimethylolpropane triglycidyl ether can also improve the toughness of the PET composite material.
2. The addition of the clay can improve the crystallization rate of the composite material, so as to improve the strength and toughness of the composite material, but the clay is easy to agglomerate.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the modified PET composite material comprises the following steps:
60 parts of PET, 30 parts of PC, 8 parts of trimethylolpropane triglycidyl ether, 0.5 part of antioxidant TNP, 4 parts of modified clay and 1 part of ethylene bis-stearamide are added into a double-screw extruder, and the mixture is subjected to melt extrusion granulation to obtain a composite material; the processing technology conditions of the double-screw extruder are as follows: the temperature of the first area is 190 ℃; the temperature of the second region is 210 ℃; the temperature of the third region is 230 ℃; the temperature of the fourth area is 255 ℃; the temperature of the fifth area is 265 ℃; the temperature of the six areas is 255 ℃; seven-zone temperature 250 ℃; the temperature of the eighth zone is 240 ℃; the temperature of the machine head is 255 ℃, and the rotating speed of the screw is 250rpm;
the preparation method of the modified clay comprises the following steps:
a1, adding 20g of clay into 80g of water, and mixing to obtain a mixture I;
a2, adding 1g of p-ethoxyformylphenyl propionaldehyde and 2g of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the mixture, heating to 80 ℃, and treating for 3 hours to obtain a mixture II;
a3, carrying out vacuum filtration on the mixture II, washing with absolute ethyl alcohol, and drying at 110 ℃ for 3 hours to obtain the modified clay.
Example 2
The preparation method of the modified PET composite material comprises the following steps:
70 parts of PET, 40 parts of PC, 12 parts of trimethylolpropane triglycidyl ether, 1 part of antioxidant 1010, 8 parts of modified clay and 2 parts of pentaerythritol stearate are added into a double-screw extruder, and the mixture is subjected to melt extrusion granulation to obtain a composite material; the processing technology conditions of the double-screw extruder are as follows: the temperature of the first area is 200 ℃; the temperature of the second area is 220 ℃; the temperature of the third region is 250 ℃; the temperature of the fourth region is 265 ℃; the temperature of the fifth area is 275 ℃; the temperature of the six areas is 265 ℃; seven-zone temperature 260 ℃; the temperature of the eighth zone is 250 ℃; the temperature of the machine head is 270 ℃, and the rotating speed of the screw is 350rpm;
the preparation method of the modified clay comprises the following steps:
a1, adding 25g of clay into 75g of water and mixing to obtain a mixture I;
a2, adding 2g of p-ethoxyformylphenyl propionaldehyde and 4g of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the mixture, heating to 100 ℃, and treating for 2 hours to obtain a mixture II;
a3, carrying out vacuum filtration on the mixture II, washing with absolute ethyl alcohol, and drying at 110 ℃ for 3 hours to obtain the modified clay.
Example 3
The preparation method of the modified PET composite material comprises the following steps:
adding 65 parts of PET, 35 parts of PC, 10 parts of trimethylolpropane triglycidyl ether, 0.6 part of antioxidant TPP, 7 parts of modified clay and 1.5 parts of pentaerythritol stearate into a double-screw extruder, and carrying out melt extrusion granulation to obtain a composite material; the processing technology conditions of the double-screw extruder are as follows: the temperature of a first area is 195 ℃; the temperature of the second area is 215 ℃; the temperature of the third region is 240 ℃; the temperature of the fourth region is 260 ℃; the temperature of the fifth area is 270 ℃; the temperature of the six areas is 260 ℃; seven-zone temperature 255 ℃; the temperature of the eighth zone is 245 ℃; the temperature of the machine head is 260 ℃ and the rotating speed of the screw rod is 300rpm;
the preparation method of the modified clay comprises the following steps:
a1, adding 23g of clay into 77g of water, and mixing to obtain a mixture I;
a2, adding 1.5g of p-ethoxyformylphenyl propionaldehyde and 3g of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the mixture, heating to 90 ℃, and treating for 2.5h to obtain a mixture II;
a3, carrying out vacuum filtration on the mixture II, washing with absolute ethyl alcohol, and drying at 110 ℃ for 3 hours to obtain the modified clay.
Example 4
The difference in example 4 compared with example 1 is that the amount of p-ethoxyformylphenylpropionaldehyde added is 2g.
Example 5
Example 5 differs from example 1 in that the amount of isopropyl tris (dioctyl pyrophosphoryloxy) titanate added is 3g.
Comparative example 1
Comparative example 1 the trimethylolpropane triglycidyl ether was replaced with an equivalent amount of glycidyl methacrylate as compared with example 1, except that the same as in example 1 was used.
Comparative example 2
Comparative example 2 was substituted for p-ethoxyformylphenylpropionaldehyde with an equivalent amount of isopropyl tri (dioctyl pyrophosphoryl oxy) titanate as in example 1, except that the equivalent amount was the same as in example 1.
Comparative example 3
Comparative example 3 the isopropyl tris (dioctyl pyrophosphoryloxy) titanate was replaced with an equivalent amount of p-ethoxyformylphenyl propionaldehyde as compared to example 1, except that example 1 was followed.
Comparative example 4
Comparative example 4 is different from example 1 in that the clay is not subjected to the modification treatment.
Comparative example 5
Comparative example 5 differs from example 1 in that trimethylolpropane triglycidyl ether was 14 parts.
Comparative example 6
Comparative example 6 differs from example 1 in that trimethylolpropane triglycidyl ether was 6 parts.
Performance testing
The modified PET composites prepared in examples 1 to 5 and comparative examples 1 to 6 were molded into bars by an injection molding machine, and the performance was measured, and the test results are shown in Table 1.
Tensile strength: the test conditions were 50mm/min, measured according to ASTM D638; notched Izod impact Strength: the test conditions were as follows, measured according to astm d 256: a notched cantilever impact bar with a thickness of 3.2mm is used, and the temperature is 23℃: flexural strength: the test conditions were 2mm/min, measured according to ASTMD 790.
TABLE 1 results of Performance test of modified PET composites of examples 1-5 and comparative examples 1-6
Comparative example 1 replaces trimethylolpropane triglycidyl ether with an equal amount of glycidyl methacrylate, comparative example 5 increases the amount of trimethylolpropane triglycidyl ether added, comparative example 6 decreases the amount of trimethylolpropane triglycidyl ether added, and as a result, both the tensile strength, impact strength and flexural strength of comparative example 1 and comparative examples 5-6 are lower than those of example 1, indicating that the mechanical properties of the composite material are improved to a higher extent than those of glycidyl methacrylate, and that increasing or decreasing the amount of trimethylolpropane triglycidyl ether added results in a decrease in the mechanical properties of the composite material.
Compared with example 1, the mechanical properties of the composite materials prepared in comparative examples 2-4 are lower than those of example 1, as a result of the fact that only isopropyl tri (dioctyl pyrophosphoryl) titanate is added, only p-ethoxyformylphenylpropionaldehyde is added, and the mechanical properties of the composite materials prepared in comparative example 4 are not modified by the clay, so that the effect of treating the clay by adding isopropyl tri (dioctyl pyrophosphoryl) titanate and p-ethoxyformylphenylpropionaldehyde simultaneously is better than that of adding either isopropyl tri (dioctyl pyrophosphoryl) titanate and p-ethoxyformylphenylpropionaldehyde.
Compared with example 1, the mass ratio of the p-ethoxyformylbenzenepropanal to the propyltri (dioctyl pyrophosphoryl) titanate in example 4 is 1:1, the mass ratio of the p-ethoxyformylbenzenepropanal to the propyltri (dioctyl pyrophosphoryl) titanate in example 5 is 1:3, and as a result, the mechanical properties of the composite materials prepared in examples 4-5 are lower than those of example 1, and the mechanical properties of the composite materials prepared in example 4-5 are optimal when the mass ratio of the p-ethoxyformylbenzenepropanal to the propyltri (dioctyl pyrophosphoryl) titanate is 1:2.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (6)
1. The modified PET composite material is characterized by comprising the following components in parts by weight: 60-70 parts of PET, 30-40 parts of PC, 8-12 parts of trimethylolpropane triglycidyl ether, 0.5-1 part of antioxidant, 4-8 parts of modified clay and 1-2 parts of lubricant;
the modified clay is obtained by treating clay with p-ethoxyformylphenyl propionaldehyde and isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate;
the preparation method of the modified clay comprises the following steps:
a1, mixing clay and water to obtain a mixture I;
a2, adding p-ethoxyformylphenyl propionaldehyde and isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the mixture I, heating to 80-100 ℃, and treating for 2-3h to obtain a mixture II;
a3, filtering, washing and drying the mixture II to obtain modified clay;
the mass content of the clay in the mixture I in the A1 is 20-25%;
the adding amount of the p-ethoxyformylbenzene propionaldehyde in the A2 is 1-2% of the mass of the mixture I, and the adding amount of the isopropyl tri (dioctyl pyrophosphoryloxy) titanate in the A2 is 2-4% of the mass of the mixture I.
2. A modified PET composite as claimed in claim 1 wherein the antioxidant comprises one or more of antioxidant 1010, antioxidant TNP and antioxidant TPP.
3. A modified PET composite as in claim 1 wherein the lubricant comprises one or more of pentaerythritol stearate, ethylene bis-stearamide.
4. The modified PET composite of claim 1, wherein the mass ratio of p-ethoxyformylbenzene propionaldehyde to isopropyl tri (dioctyl pyrophosphoryloxy) titanate in A2 is 1:2.
5. The method for preparing a modified PET composite according to claim 1, comprising the steps of: mixing PET, PC, trimethylolpropane triglycidyl ether, an antioxidant, modified clay and a lubricant, and extruding the mixture through an extruder to obtain the modified PET composite material.
6. The method for preparing a modified PET composite according to claim 5, wherein the extruder is a twin-screw extruder, and the process parameters of the twin-screw extruder are as follows: the temperature of the first area is 190-200 ℃; the temperature of the second area is 210-220 ℃; the temperature of the third region is 230-250 ℃; the temperature of the fourth area is 255-265 ℃; the temperature of the fifth area is 265-275 ℃; the temperature of the six areas is 255-265 ℃; the temperature of the seventh area is 250-260 ℃; the temperature of the eighth zone is 240-250 ℃; the temperature of the machine head is 255-270 ℃, and the rotating speed of the screw is 250-350rpm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101495569A (en) * | 2006-07-28 | 2009-07-29 | 帝人株式会社 | Resin composition, method for producing the same and molded article |
| CN103172988A (en) * | 2013-03-25 | 2013-06-26 | 山东汇盈新材料科技有限公司 | Method for increasing capacity of biodegradable polyester blend film |
| WO2021253772A1 (en) * | 2020-06-15 | 2021-12-23 | 金发科技股份有限公司 | Low-smoke density high-performance halogen-free flame-retardant reinforced pbt composite and preparation method therefor |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101495569A (en) * | 2006-07-28 | 2009-07-29 | 帝人株式会社 | Resin composition, method for producing the same and molded article |
| CN103172988A (en) * | 2013-03-25 | 2013-06-26 | 山东汇盈新材料科技有限公司 | Method for increasing capacity of biodegradable polyester blend film |
| WO2021253772A1 (en) * | 2020-06-15 | 2021-12-23 | 金发科技股份有限公司 | Low-smoke density high-performance halogen-free flame-retardant reinforced pbt composite and preparation method therefor |
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