CN114806190A - TPV material composition, preparation and application thereof - Google Patents
TPV material composition, preparation and application thereof Download PDFInfo
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- CN114806190A CN114806190A CN202210238308.4A CN202210238308A CN114806190A CN 114806190 A CN114806190 A CN 114806190A CN 202210238308 A CN202210238308 A CN 202210238308A CN 114806190 A CN114806190 A CN 114806190A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention relates to a TPV material composition, a preparation method and an application thereof, wherein the TPV material composition comprises the following components: the low-melting PP resin, the high-melting PP resin, the low-Mooney EPDM rubber, the high-Mooney EPDM rubber, paraffin oil, a vulcanizing agent, a vulcanization accelerator, an antioxidant, a light stabilizer and a lubricant. According to the invention, the TPV material with high fluidity and low glossiness is prepared through the synergistic interaction of the components.
Description
Technical Field
The invention belongs to the field of thermoplastic elastomers, and particularly relates to a TPV material composition, and preparation and application thereof.
Background
The thermoplastic vulcanizate (TPV) has the advantages of excellent low temperature resistance, good touch, low high-temperature compression set, good heat resistance and weather resistance, and the like, and is widely used for automobile interior and exterior parts. However, for larger interior trim parts, a material with higher flow properties is required for better formability, while lower gloss can give a higher end of the interior trim feel.
The TPV product is a high-molecular elastomer material prepared by taking plastic as a continuous phase and rubber as a disperse phase and adopting a PP and EPDM dynamic vulcanization process, and is difficult to simultaneously have high fluidity and low glossiness for a TPV product with low hardness.
Disclosure of Invention
Based on the defects in the prior art, the technical problem to be solved by the invention is to provide a TPV material composition, and a preparation method and an application thereof, wherein the TPV material composition has high fluidity and low glossiness.
The invention provides a TPV material composition, which comprises the following components in parts by weight:
wherein the low-melting-index PP resin has a melt index of 230 ℃ and a melt index of less than or equal to 2g/10min under the condition of 2.16 kg;
the high-melt-index PP resin has a melt index of 230 ℃ and a melt index of 30-50 g/10min under the condition of 2.16 kg;
the melt indexes of the low-melt-index PP resin and the high-melt-index PP resin are detected according to an ISO 1133-1-2011 standard method.
The Mooney viscosity of the low-Mooney EPDM rubber is ML (1+4) at 125 ℃ of 40-70;
the Mooney viscosity of the high-Mooney EPDM rubber is ML (1+4) at 125 ℃ of 75-120.
The Mooney viscosities of the above-mentioned low-Mooney EPDM rubber and high-Mooney EPDM rubber were measured according to ISO 289-1-2014 standard method.
Preferably, the low-melting-index PP resin has a melt index of 230 ℃ and a melt index of less than or equal to 1g/10min under the condition of 2.16 kg.
The inventor researches and discovers that when the melt index of the low-melt-index PP resin is less than or equal to 1g/10min and the melt index of the high-melt-index PP resin is 30-50 g/10min, the flowability and the glossiness of the TPV material are lower.
Preferably, the ENB weight percentage content of the low-Mooney EPDM rubber is 3.5-6.5 wt%; the weight percentage content of ENB of the high-Mooney EPDM rubber is 3.5-6.5 wt%.
More preferably, the ENB weight percentage content of the low-Mooney EPDM rubber is 4-5.5 wt%.
More preferably, the ENB weight percentage content of the high-Mooney EPDM rubber is 4-5.5 wt%.
The inventor finds that when the Mooney viscosity of the EPDM rubber is lower, the molecular weight of the EPDM rubber is lower, which is beneficial to blending with the PP material, and when the Mooney viscosity of the EPDM rubber is higher, the molecular weight of the EPDM rubber is higher, which is beneficial to reducing the gloss of the material. The low melting point means that the PP resin is added in an amount of 8-12 parts by weight, the viscosity of the low melting point PP resin can be closer to that of low-Mooney EPDM rubber, and the low melting point PP resin is beneficial to mixing and dispersing the PP resin and the EPDM rubber.
The EPDM rubber has the advantages that the ENB content influences the vulcanization speed and the performance of vulcanized rubber, the rubber vulcanization speed is high due to the ENB content, scorching is easy to generate, the rubber is not beneficial to shearing and crushing into fine sizes, the rubber phase size is overlarge, the comprehensive mechanical property of the material is poor, the ENB content is too low, the rubber vulcanization speed is too low, the rubber cannot be fully vulcanized within the retention time of a screw, the comprehensive mechanical property of the material is not good, when the ENB content in the EPDM is 3.5-6.5%, the rubber vulcanization speed is proper, the crushing size of the vulcanized rubber is small, and the comprehensive performance of the material is good.
Preferably, the paraffin oil is high-flash-point paraffin oil without polycyclic aromatic hydrocarbon, and the open flash point is more than or equal to 260 ℃.
The open flash point was tested according to the GB/T267-1988 standard method with a temperature rise rate of 1 ℃/min.
The paraffin oil does not contain polycyclic aromatic hydrocarbon, and is more environment-friendly. The open flash point is higher, and the prepared TPV product has better heat resistance and lower haze.
More preferably, the open flash point of the paraffin oil is 265-300 ℃.
Preferably, the vulcanizing agent is a peroxide type vulcanizing agent.
Preferably, the peroxide vulcanizing agent is one or more of tert-butyl peroxyisopropylcarbonate, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and di-tert-butylperoxycumyl.
Preferably, the vulcanization accelerator is one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, triallyl isocyanurate and diphenylmethane maleimide.
Preferably, the antioxidant is one or more of antioxidant 1010, antioxidant 1076, antioxidant 1790, antioxidant 168, antioxidant DLTP and antioxidant 626.
Preferably, the light stabilizer is one or more of hindered amine light stabilizer and triazine light stabilizer.
Further preferably, the light stabilizer is a mixture of a hindered amine light stabilizer and a triazine light stabilizer in a weight ratio of 3: 2.
Preferably, the hindered amine light stabilizer can be one or more of light stabilizer 622, light stabilizer 944, light stabilizer 783, light stabilizer 3853, light stabilizer 292 or light stabilizer 123; preferably, the triazine light stabilizer is one or more of UV-234, UV-236 or UV-237.
Preferably, the lubricant is one or more of fatty amide, stearate and polyethylene wax.
Preferably, the components comprise the following components in parts by weight:
the invention provides a preparation method of the TPV material composition, which comprises the following steps:
(1) weighing the components in parts by weight, mixing low-melting-index PP resin, high-melting-index PP resin, low-Mooney EPDM rubber, vulcanization accelerator, antioxidant, lubricant and light stabilizer, adding the mixture to a main feeding port of a double-screw extruder, adding paraffin oil into a section 3 screw cylinder of the double-screw extruder, and carrying out melt mixing and extrusion granulation to obtain a TPV (thermoplastic vulcanizate) first-step material;
(2) and (2) mixing the TPV primary material prepared in the step (1) and high Mooney EPDM, adding the mixture into a double-screw extruder, adding a vulcanizing agent into a section 6 screw cylinder of the double-screw extruder, and performing melt extrusion granulation to obtain the TPV material.
Preferably, the screw rotating speed of the double-screw extruder in the step (1) is 350-450 r/min, and the melt mixing temperature is 120-180 ℃;
preferably, the screw rotating speed of the double-screw extruder in the step (2) is 400-500 r/min, and the melt mixing temperature is 120-200 ℃;
preferably, in the step (2), water is injected into the 10 th section of screw cylinder of the double-screw extruder, the injection weight of the water is 5-10% of the weight of the TPV one-step material, the 13 th section of screw cylinder of the double-screw extruder is vacuumized, and the vacuum degree is less than or equal to 0.09 MPa.
The invention provides an application of the TPV material composition in automotive interior trim.
The TPV material with high fluidity and low gloss is prepared by the mutual cooperation and synergistic effect of the components of PP resin with low melt index, PP resin with high melt index, EPDM with low viscosity, EPDM rubber with high viscosity and the like;
the high-melt-index PP resin and the low-melt-index PP resin form a bimodal system, the viscosity difference between the PP resin and the EPDM is reduced, a small amount of high-weight EPDM is added in the dynamic vulcanization process to participate in the dynamic vulcanization, and the aim is to form a small amount of large EPDM phase structure, so that low glossiness is realized.
Advantageous effects
The TPV material composition has high fluidity, low glossiness and ageing resistance.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
1. TABLE 1 raw materials referred to in examples and comparative examples
The lubricant, vulcanizing agent, vulcanization accelerator, antioxidant and light stabilizer used in the parallel experiment are all the same commercial products.
2. The performance of the TPV materials prepared in the examples and the comparative examples is tested, and the test method is as follows:
material flow properties describe the ability of the melt to fill the mold cavity and the method of measurement is melt index measurement.
Melt index:
the test condition is 230 ℃ and 2.16kg according to the ISO 1133-1-2011 standard method.
Gloss:
the test condition is 60 DEG angle gloss according to the test method of ISO 2813-2014 standard.
Gloss after aging:
firstly, carrying out heat aging according to the ISO 188-.
Examples 1 to 11
The components are weighed according to the parts by weight, and are specifically shown in table 2.
(1) Mixing low-melting-index PP resin, high-melting-index PP resin, low-Mooney EPDM rubber, a vulcanization accelerator, an antioxidant, a lubricant and a light stabilizer, adding the mixture to a main feeding port of a double-screw extruder, adding paraffin oil into a section 3 screw cylinder of the double-screw extruder, and carrying out melt mixing, extrusion and granulation to obtain a TPV (thermoplastic vulcanizate) primary material, wherein the rotating speed of a screw of the double-screw extruder is 350-450 r/min, and the melt mixing temperature is 120-180 ℃;
(2) mixing the TPV one-step material and high-Mooney EPDM rubber, adding the mixture into a double-screw extruder, adding a vulcanizing agent into a 6 th screw barrel of the double-screw extruder, injecting water into a 10 th screw barrel of the double-screw extruder, wherein the injection weight of the water is 5-10% of the weight of the TPV one-step material, vacuumizing the 13 th screw barrel of the double-screw extruder, and the vacuum degree is less than or equal to 0.09 MPa; performing melt extrusion granulation to obtain the TPV material; wherein the screw rotating speed of the double-screw extruder is 400-550 r/min, and the melting and mixing temperature is 120-200 ℃.
TABLE 2 component content (parts by weight) of TPV materials of examples 1 to 11
Comparative examples 1 to 8
The components are weighed according to the parts by weight, and the preparation method is the same as the example as shown in the table 3.
TABLE 3 component contents (parts by weight) of TPV materials of comparative examples 1 to 8
The tables for testing the properties of the TPVs obtained in examples 1 to 11 are shown in Table 4.
TABLE 4 test results of examples 1 to 11
The TPVs obtained in comparative examples 1 to 8 were subjected to the property test shown in Table 5.
TABLE 5 test results for comparative examples 1 to 8
Compared with the example 1, the comparative examples 1-4 of the invention can ensure that the TPV material composition has high fluidity, low gloss and ageing resistance simultaneously through the synergistic combination of the low-melt-index PP resin, the high-melt-index PP resin, the low-viscosity EPDM and the high-viscosity EPDM rubber.
Claims (10)
1. The TPV material composition is characterized by comprising the following components in parts by weight:
wherein the low-melting-index PP resin has a melt index of 230 ℃ and a melt index of less than or equal to 2g/10min under the condition of 2.16 kg;
the high-melt-index PP resin has a melt index of 230 ℃ and a melt index of 30-50 g/10min under the condition of 2.16 kg;
the Mooney viscosity of the low-Mooney EPDM rubber is ML (1+4) at 125 ℃ of 40-70;
the Mooney viscosity of the high-Mooney EPDM rubber is ML (1+4) at 125 ℃ of 75-120.
2. The composition as claimed in claim 1, wherein the low-melting-index PP resin has a melt index of 230 ℃ or less than 1g/10min under 2.16 kg.
3. The composition of claim 1 wherein the low mooney EPDM rubber has 3.5 to 6.5 wt.% ENB; the weight percentage content of ENB of the high-Mooney EPDM rubber is 3.5-6.5 wt%.
4. The composition of claim 1, wherein the paraffinic oil has an open flash point of 260 ℃.
5. The composition according to claim 1, characterized in that said vulcanizing agent is a peroxide type vulcanizing agent; the peroxide vulcanizing agent is one or more of tert-butyl peroxyisopropylcarbonate, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and di-tert-butylperoxycumine; the vulcanization accelerator is one or more of trimethylolpropane triacrylate, trimethylolpropane trimethacrylate, triallyl isocyanurate and diphenylmethane maleimide.
6. The composition of claim 1, wherein the antioxidant is one or more of antioxidant 1010, antioxidant 1076, antioxidant 1790, antioxidant 168, antioxidant DLTP, and antioxidant 626; the light stabilizer is one or more of hindered amine light stabilizer and triazine light stabilizer; the lubricant is one or more of fatty amide, stearate and polyethylene wax.
7. The composition according to claim 1, which comprises the following components in parts by weight:
8. a method of making a TPV material composition as claimed in any one of claims 1 to 7, comprising:
(1) weighing the components in parts by weight, mixing low-melt-index PP resin, high-melt-index PP resin, low-Mooney EPDM rubber, vulcanization accelerator, antioxidant, lubricant and light stabilizer, adding the mixture into a main feeding port of a double-screw extruder, adding paraffin oil into a section 3 screw cylinder of the double-screw extruder, and carrying out melt mixing and extrusion granulation to obtain a TPV (thermoplastic vulcanizate) primary material;
(2) and (2) mixing the TPV primary material prepared in the step (1) and high Mooney EPDM, adding the mixture into a double-screw extruder, adding a vulcanizing agent into a section 6 screw cylinder of the double-screw extruder, and performing melt extrusion granulation to obtain the TPV material.
9. The preparation method according to claim 8, wherein the screw rotation speed of the twin-screw extruder in the step (1) is 350-450 r/min, and the melt mixing temperature is 120-180 ℃; in the step (2), the screw rotating speed of the double-screw extruder is 400-500 r/min, and the melting and mixing temperature is 120-200 ℃; and (2) injecting water into a 10 th section of screw cylinder of the double-screw extruder, wherein the injection weight of the water is 5-10% of the weight of the TPV one-step material, and vacuumizing a 13 th section of screw cylinder of the double-screw extruder, wherein the vacuum degree is less than or equal to 0.09 MPa.
10. Use of the TPV material composition of claim 1 in automotive interiors.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116003919A (en) * | 2022-12-29 | 2023-04-25 | 金发科技股份有限公司 | TPV material fast bonded with alpha-ethyl cyanoacrylate adhesive |
| CN116063798A (en) * | 2022-12-29 | 2023-05-05 | 金发科技股份有限公司 | High Wen Kailian-resistant TPV material and preparation method and application thereof |
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| CN116063798A (en) * | 2022-12-29 | 2023-05-05 | 金发科技股份有限公司 | High Wen Kailian-resistant TPV material and preparation method and application thereof |
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