CN112852060A - Low-density composite material and preparation method and application thereof - Google Patents
Low-density composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a low-density composite material and a preparation method and application thereof, belonging to the technical field of composite materials. The invention provides a low-density composite material, which comprises preparation raw materials and an additive; the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer; the additives include dispersants and nucleating agents. The composite material provided by the invention takes the polypropylene, the coupling agent modified ZSM-5 molecular sieve and the polyolefin elastomer as the preparation raw materials, and the proportion of the three raw materials is reasonably controlled, so that the obtained composite material has the advantages of light weight and high strength, and can be used in the field of automobiles.
Description
Technical Field
The invention belongs to the field of preparation of lightweight automobile materials, and particularly relates to a low-density composite material and a preparation method and application thereof.
Background
The existing method for lightening the automobile mainly comprises the steps of optimizing the structural design of the automobile and searching for a suitable substitute material, wherein the optimization of the automobile structure usually needs to develop and design a new structure which is more perfect. Among them, a lightweight alternative material is one of important weight reduction means. According to incomplete statistics, about 70-120 kg of the car body is plastic, polypropylene is the most used plastic for automobile structural parts, parts and accessories, and accounts for about 80% of the plastic for the car, and is 56-96 kg. Therefore, the PP is modified to reduce the density of the PP composite material, and the method has important significance for automobile light weight.
At present, the prior literature at home and abroad reports that talcum powder, mica, hollow glass microspheres, glass fibers and whiskers are adopted to modify polypropylene to prepare various low-density polypropylene composite materials. The PP/glass fiber composite material has good mechanical property and the density of the PP/glass fiber composite material is 1.5g/cm3～2.0g/cm3(＞1.0g/cm3) Does not meet the low density requirement of the polypropylene composite material; the density of the low-density polypropylene composite material prepared by filling the hollow glass beads is 0.98g/cm3～1.03g/cm3Glass beads are easy to break in the material preparation stage, and other auxiliary agents are needed for compensation and toughening; the density of the whisker filled polypropylene material is 0.99g/cm3～1.02g/cm3And the whisker still has a light-weight space, and has small surface area, small contact surface with resin, poor compatibility of two phases, increased content, aggregated whisker and reduced mechanical property of the composite material. Therefore, on the premise of ensuring the mechanical property, the proper modifier is selected to reduce the density of the polypropylene composite material.
At present, no research report that the molecular sieve is added into polypropylene as a low-density polypropylene modifier exists, and the low-density polypropylene composite material in the market has a space for continuously lightening the weight.
Disclosure of Invention
In view of the above, the invention aims to provide a low-density composite material, and a preparation method and an application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a low-density composite material, which comprises preparation raw materials and an additive;
the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer;
the additives include dispersants and nucleating agents.
Preferably, the dispersant is dispersant TAS-2A; the nucleating agent is a nucleating agent HPN-68L.
Preferably, the mass of the dispersing agent is 0.1-0.5% of the mass of the preparation raw material; the mass of the nucleating agent is 0.05-0.1% of that of the preparation raw material.
Preferably, the mass of the dispersing agent is 0.2 percent of the mass of the preparation raw material; the mass of the nucleating agent is 0.08 percent of the mass of the preparation raw material.
Preferably, the coupling agent modified ZSM-5 molecular sieve has a median particle size D50 of 1.06 μm.
Preferably, the coupling agent modified ZSM-5 molecular sieve is prepared by a method comprising the following steps:
mixing absolute ethyl alcohol and a coupling agent KH-560, and hydrolyzing under the condition that the pH value is 4 to obtain hydrolyzed liquid;
and mixing the hydrolysis feed liquid with the ZSM-5 molecular sieve, and carrying out modification reaction to obtain the coupling agent modified ZSM-5 molecular sieve.
Preferably, the dosage ratio of the absolute ethyl alcohol to the coupling agent KH-560 to the ZSM-5 molecular sieve is 100 mL: 1mL of: 15 g.
The invention also provides a preparation method of the low-density composite material, which comprises the following steps:
and melting and extruding the polypropylene, the coupling agent modified ZSM-5 molecular sieve, the polyolefin elastomer, the dispersing agent and the nucleating agent to obtain the low-density composite material.
Preferably, the melt extrusion is carried out in a twin screw extruder having a first zone temperature of 190 ℃, a second zone temperature of 195 ℃, a third zone temperature of 195 ℃ and a fourth zone temperature of 190 ℃.
The invention also provides application of the low-density composite material in the technical scheme or the low-density composite material prepared by the preparation method in the technical scheme in the field of automobiles.
The invention provides a low-density composite material, which comprises preparation raw materials and an additive; the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer; the additives include dispersants and nucleating agents. The composite material provided by the invention takes the polypropylene, the coupling agent modified ZSM-5 molecular sieve and the polyolefin elastomer as the preparation raw materials, and the proportion of the three raw materials is reasonably controlled, so that the obtained composite material has the advantages of light weight and high strength, and can be used in the field of automobiles.
The data of the examples show that: the density of the low-density composite material provided by the invention is 0.908-0.97 g/cm3Compared with the traditional mature PP + EPDM-T20 composite material, the density is reduced by 7-13%, and the weight is light; the bending strength is 54.05-58.47 MPa, the total strength is improved by 80-95% compared with that of the traditional mature PP + EPDM-T20 composite material, and the mechanical strength is high.
Detailed Description
The invention provides a low-density composite material, which comprises preparation raw materials and an additive; the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer; the additives include dispersants and nucleating agents.
In the present invention, the starting materials used in the present invention are preferably commercially available products unless otherwise specified.
The raw materials for preparing the low-density composite material comprise 45-85 mass percent of polypropylene, and the number average molecular weight of the polypropylene is preferably excellentIs selected to be 5 × 104～7×104。
The preparation raw material of the low-density composite material comprises 3-15% by mass of a coupling agent modified ZSM-5 molecular sieve, and the median particle size D50 of the coupling agent modified ZSM-5 molecular sieve is preferably 1.06 mu m. In the present invention, the coupling agent modified ZSM-5 molecular sieve is preferably prepared by a method comprising the steps of:
mixing absolute ethyl alcohol and a coupling agent KH-560, and hydrolyzing under the condition that the pH value is 4 to obtain hydrolyzed liquid;
and mixing the hydrolysis feed liquid with the ZSM-5 molecular sieve, and carrying out modification reaction to obtain the coupling agent modified ZSM-5 molecular sieve.
The invention mixes absolute ethyl alcohol and coupling agent KH-560, hydrolyzes under the condition of pH 4, and obtains hydrolyzed liquid. The pH adjusting agent of the present invention is not particularly limited as long as the pH of the mixed solution obtained by mixing absolute ethanol and the coupling agent KH-560 can be adjusted to 4. In the invention, the anhydrous ethanol and the coupling agent KH-560 are preferably mixed in a mode of: adjusting the pH value of absolute ethyl alcohol to 4, then adding a coupling agent KH-560, and hydrolyzing; the hydrolysis time is preferably 5 min.
After hydrolysis feed liquid is obtained, the hydrolysis feed liquid and the ZSM-5 molecular sieve are mixed for modification reaction to obtain the coupling agent modified ZSM-5 molecular sieve.
In the invention, the dosage ratio of the absolute ethyl alcohol, the coupling agent KH-560 and the ZSM-5 molecular sieve is preferably 100 mL: 1mL of: 15 g.
In the invention, the hydrolysis feed liquid and the molecular sieve ZSM-5 are preferably mixed under the condition of stirring, and the stirring speed is not particularly limited. In the present invention, the temperature of the modification reaction is preferably 60 ℃ and the time is preferably 0.5 h.
After the modification reaction is finished, the method preferably further comprises the steps of cooling the obtained modification reaction feed liquid to room temperature, cleaning the cooled modification reaction feed liquid with ethanol, filtering, drying and grinding after the cleaning is finished, so as to obtain the coupling agent modified ZSM-5 molecular sieve. The number of times of the washing is not particularly limited, and the coupling agent KH-560 physically adsorbed on the surface of the ZSM-5 molecular sieve can be completely removed. In the invention, the drying temperature is preferably 100 ℃, and the drying time is preferably 24 hours; the grinding mode and parameters are not particularly limited, and the modified ZSM-5 molecular sieve with the target size can be obtained finally.
The raw materials for preparing the low-density composite material comprise 10-40% by mass of Polyolefin (PEO) elastomer, and the melt flow index of the PEO elastomer is preferably 0.5g/10 min. In the invention, the POE elastomer can improve the toughness of the low-density composite material.
The present invention provides a low density composite comprising an additive; the additive comprises a dispersant and a nucleating agent; the dispersant is preferably dispersant TAS-2A; the mass of the dispersing agent is preferably 0.1-0.5% of that of the preparation raw material, and is further preferably 0.2%; in the invention, the dispersing agent can improve the dispersion uniformity of the raw materials and improve the surface smoothness of the composite material.
In the present invention, the nucleating agent is preferably a nucleating agent HPN-68L; the mass of the nucleating agent is preferably 0.05-0.1% of that of the preparation raw material, and more preferably 0.08% of that of the preparation raw material. In the invention, the addition of the nucleating agent can control the shrinkage rate of the low-density composite material and make the tissue structure of the material uniform.
In a specific embodiment of the present invention, the raw materials for preparing the low-density composite material preferably include the following components in percentage by mass: the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer; the mass of the dispersant TAS-2A is 0.2 percent of the mass of the preparation raw material; the nucleating agent HPN-68L accounts for 0.08 percent of the mass of the raw materials for preparation.
The invention also provides a preparation method of the low-density composite material, which comprises the following steps:
and melting and extruding the polypropylene, the coupling agent modified ZSM-5 molecular sieve, the polyolefin elastomer, the dispersing agent and the nucleating agent to obtain the low-density composite material.
In the present invention, the polypropylene, the coupling agent modified ZSM-5 molecular sieve and the polyolefin elastomer are preferably subjected to a drying treatment before use: the drying treatment temperature of the polypropylene is preferably 80 ℃, and the time is preferably 8 h; the drying treatment temperature of the coupling agent modified ZSM-5 molecular sieve is preferably 110 ℃, and the time is preferably 8 h; the drying treatment temperature of the polyolefin elastomer is 50 ℃, and the drying treatment time is 8 h.
In the present invention, the melt extrusion is preferably carried out in a twin screw extruder, the temperature of the first zone of which is preferably 190 ℃, the temperature of the second zone of which is preferably 195 ℃, the temperature of the third zone of which is preferably 195 ℃ and the temperature of the fourth zone of which is preferably 190 ℃.
The invention also provides the application of the low-density composite material in the technical scheme or the low-density composite material prepared by the preparation method in the technical scheme in the field of automobiles. In the invention, when the low-density composite material is applied to the field of automobiles, the mode or form of the application is not particularly limited, and the mode or form can be selected according to actual conditions.
The low-density composite material provided by the present invention, the preparation method and the application thereof are described in detail with reference to the following examples, but they should not be construed as limiting the scope of the present invention.
Examples
The formulations of the composites of examples 1-7 and comparative example 1 are shown in Table 1.
TABLE 1 formulations of composites of examples 1-7 and comparative example 1
Wherein, the mass percentage of the TAS-2A and the HPN-68L is relative to the total mass of the iPP, the POE and the M-ZSM-5.
The preparation method of the coupling agent modified molecular sieve (M-ZSM-5 for short) comprises the following steps:
adjusting pH to 4 with 100mL of absolute ethanol, adding 1mL of KH-560 into absolute ethanol, standing for hydrolysis for 5min, adding 15g of ZSM-5 molecular sieve at a constant temperature of 60 ℃, reacting for 0.5h, standing for cooling for a period of time, repeatedly washing the reacted suspension with ethanol until KH-560 physically adsorbed on the surface of the superfine molecular sieve is completely removed, drying for 24h at 100 ℃, grinding, and sieving to obtain M-ZSM-5.
The low-density composite materials obtained in examples 1 to 5 and comparative example 1 were named iPP/3% M-ZSM-5/POE, iPP/5% M-ZSM-5/POE, iPP/10% M-ZSM-5/POE, iPP/12% M-ZSM-5/POE, iPP/15% M-ZSM-5/POE, and iPP, respectively.
Performance testing
Note: the density is measured according to GB 1033-86 test method for density and relative density of plastics; shrinkage was measured according to GB/T17037.4-2003 part 4 of the preparation of injection molded specimens of thermoplastic plastics materials, determination of the mold shrinkage; tensile Properties test determination of tensile Properties of plastics part 2 according to GB/T1040.2-2006: test conditions for molded and extruded plastics "; the bending property is implemented according to the standard of GB/T9341-; the impact strength was measured according to GB/T1843-2008 "determination of impact Strength of Plastic cantilever". The tests were all at room temperature. The impact strength is notch impact strength. The results obtained are shown in Table 2.
TABLE 2 Performance test results of the low-density composites obtained in examples 1 to 7 and comparative example 1
As can be seen from table 2: the density of the low density composite material gradually increases with the increase of the content of the M-ZSM-5. When the mass content of M-ZSM-5 was 5 wt% (example 2), the density of the corresponding iPP/5% M-ZSM-5/POE low density composite material was 0.920g/cm3The density is higher than that of the traditional mature PP + EPDM-T20 composite material (1.04 g/cm)3) The reduction is 11.5%; when the content of the M-ZSM-5 is less than or equal to 15wt percent, the density of the low-density composite material is less than 0.968g/cm3The composite material has obvious weight reducing effect.
After M-ZSM-5, POE and an anti-shrinkage nucleating agent HPN-68L are added into the iPP, the shrinkage rate of the low-density composite material is about 1.0% and is smaller along with the increase of the content of the M-ZSM-5. HPN-68L and POE both have the function of reducing the shrinkage rate of iPP in a polypropylene composite material system, POE enables the crystallinity of iPP to be reduced so as to reduce the shrinkage rate, HPN-68L promotes the crystallization rate of iPP to be accelerated so as to reduce the molding shrinkage rate, and the addition of the M-ZSM-5 inorganic molecular sieve promotes the heterogeneous nucleation and crystal refinement of iPP so as to reduce the molding shrinkage rate and the post shrinkage rate of iPP, so that the shrinkage rate of the low-density composite material is controlled to be about 1.0 percent.
The tensile strength of the low-density composite material tends to decrease after increasing, when the content of M-ZSM-5 is 5 wt% (example 2), the maximum tensile strength of the iPP/5% M-ZSM-5/POE composite material is 34MPa, which is 70% higher than the tensile strength (20MPa) of the PP + EPDM-T20 composite material, and when the content of M-ZSM-5 is 15 wt% (example 5), the tensile strength of the iPP/15% M-ZSM-5/POE composite material is 31MPa, which is still 55% higher than the tensile strength of the PP + EPDM-T20 composite material. In addition, when the POE content was further increased to 30% and 40% (examples 6 and 7), the tensile strength dropped to 25 MPa.
The impact strength of the low-density composite material is in a trend of increasing firstly and then decreasing rapidly along with the increase of the content of the M-ZSM-5. When the M-ZSM-5 content was 5 wt% (example 2), the impact strength of the iPP/5% M-ZSM-5/POE low-density composite material was 30.2kJ/M2Purer iPP (24.1 kJ/m)2) The impact strength is improved by 25 percent compared with PP + EPDM-T20(25 kJ/m)2) The composite material is improved by 20.8%, which shows that the low-density composite material has high toughness. When the M-ZSM-5 content was 10 wt% (example 3), the impact strength of the iPP/10% M-ZSM-5/POE low-density composite material was 26.2kJ/M2When the POE content was further increased to 30% and 40% (examples 6 and 7), the impact strength of the low-density composite material reached 39.2kJ/m2And 58.5/kJ/m2。
The bending strength of the low-density composite material is continuously reduced along with the increase of the content of the M-ZSM-5, when the content of the M-ZSM-5 is 3 wt% (example 1), the bending strength reaches the maximum value of 58.47MPa, is improved by 95 percent compared with the bending strength (30MPa) of the PP + EPDM-T20 composite material, and is improved by nearly 1 time. When the M-ZSM-5 content was 15% (example 5), the flexural strength of the low density composite was 54.05MPa, which is still 80% higher than the PP + EPDM-T20 composite. In addition, as the POE content reached 30% and 40%, the flexural strength of the low density composite decreased, but was still above 30 MPa.
In the low-density composite material, the requirements of the automobile instrument panel and the inner door panel on the low-density composite material are completely met in the embodiments 1 to 5, wherein the requirement of the instrument panel is that the density is less than or equal to 1.06g/cm3The tensile strength is more than or equal to 20MPa, the bending strength is more than or equal to 25MPa, and the impact strength of a cantilever beam notch is more than or equal to 20kJ/m2(ii) a The requirement of the inner door panel on the composite material is that the density is less than or equal to 1.03g/cm3The melt index is more than or equal to 12g/10min, the tensile strength is more than or equal to 20MPa, and the bending strength is more than or equal to 25 MPa. Examples 6 to 7 satisfy the requirements of the front and rear bumpers of the automobile for the density of the low-density composite material being less than or equal to 1g/cm3The tensile strength is more than or equal to 17MPa, the bending strength is more than or equal to 23MPa, and the impact strength of a cantilever beam notch is more than or equal to 32kJ/m2The requirements of (1).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A low-density composite material is characterized by comprising preparation raw materials and additives;
the preparation raw materials comprise the following components in percentage by mass: 45-85% of polypropylene, 3-15% of coupling agent modified ZSM-5 molecular sieve and 10-40% of polyolefin elastomer;
the additives include dispersants and nucleating agents.
2. The low density composite of claim 1, wherein the dispersant is dispersant TAS-2A; the nucleating agent is a nucleating agent HPN-68L.
3. The low-density composite material as claimed in claim 1 or 2, wherein the mass of the dispersant is 0.1-0.5% of the mass of the raw material for preparation; the mass of the nucleating agent is 0.05-0.1% of that of the preparation raw material.
4. The low density composite of claim 3, wherein the mass of the dispersant is 0.2% of the mass of the raw materials for preparation; the mass of the nucleating agent is 0.08 percent of the mass of the preparation raw material.
5. The low density composite of claim 1, wherein the coupling agent modified ZSM-5 molecular sieve has a median particle size D50 of 1.06 μm.
6. The low density composite of claim 1 or 5, wherein the coupling agent modified ZSM-5 molecular sieve is prepared by a method comprising the steps of:
mixing absolute ethyl alcohol and a coupling agent KH-560, and hydrolyzing under the condition that the pH value is 4 to obtain hydrolyzed liquid;
and mixing the hydrolysis feed liquid with the ZSM-5 molecular sieve, and carrying out modification reaction to obtain the coupling agent modified ZSM-5 molecular sieve.
7. The low density composite according to claim 6, wherein the absolute ethanol, the coupling agent KH-560 and the ZSM-5 molecular sieve are used in a ratio of 100 mL: 1mL of: 15 g.
8. A method of making a low density composite as claimed in any one of claims 1 to 7 comprising the steps of:
and melting and extruding the polypropylene, the coupling agent modified ZSM-5 molecular sieve, the polyolefin elastomer, the dispersing agent and the nucleating agent to obtain the low-density composite material.
9. The method of claim 8, wherein the melt extrusion is performed in a twin screw extruder having a first zone temperature of 190 ℃, a second zone temperature of 195 ℃, a third zone temperature of 195 ℃ and a fourth zone temperature of 190 ℃.
10. Use of the low density composite material according to any one of claims 1 to 7 or the low density composite material prepared by the preparation method according to any one of claims 8 to 9 in the automotive field.
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| CN113698699A (en) * | 2021-07-22 | 2021-11-26 | 国家能源集团宁夏煤业有限责任公司 | Composition for producing polypropylene composite material, polypropylene composite material and preparation method and application thereof |
| CN116693971A (en) * | 2023-06-29 | 2023-09-05 | 涿州市隽诚化工有限公司 | Anti-yellowing modified composite additive for polyolefin and preparation method and application thereof |
| CN116693971B (en) * | 2023-06-29 | 2024-06-04 | 涿州市隽诚化工有限公司 | Anti-yellowing modified composite additive for polyolefin and preparation method and application thereof |
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