CN111138754A - High-fluidity and high-rigidity alloy composite material and preparation method thereof - Google Patents
High-fluidity and high-rigidity alloy composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of modified alloy composite materials, and particularly relates to a high-fluidity and high-rigidity alloy composite material and a preparation method thereof. The high-fluidity and high-rigidity alloy composite material comprises the following raw materials, by weight, 60-80% of polypropylene resin, 10-20% of polybutylene resin, 0.5-3.0% of compatilizer, 5-15% of flexibilizer, 10-30% of inorganic powder and 1-5% of auxiliary agent, so that on the premise of keeping excellent comprehensive mechanical properties, the inorganic powder is well dispersed in a base material, and meanwhile, the fluidity of the material is improved; by adopting the PP/PB crosslinking grafting compatilizer, the compatilizer has the same chain segment with the blend, so that the compatilizer has an emulsifying effect at a PP and PB phase interface, improves the compatibility of a base material polypropylene/polybutylene alloy system, ensures that the polypropylene/polybutylene alloy material has high fluidity, high dispersibility and high rigidity, realizes the injection molding of large-sized parts on a general injection molding machine, and can be widely applied to multiple fields of household appliances, automobiles and the like.
Description
Technical Field
The invention belongs to the technical field of modified alloy composite materials, and particularly relates to a high-fluidity and high-rigidity alloy composite material and a preparation method thereof.
Background
The polypropylene resin has good physical properties and moldability, has the advantages of good chemical corrosion resistance, no peculiar smell, no toxicity and the like, simultaneously has rich raw materials and low price, but has some defects, and the fluidity and the mechanical properties of products can not meet the actual requirements when large-scale finished products are molded. To solve the problems of polypropylene application, filling modification is needed. The polybutene as one kind of inert polymer has high mechanical performance, high chemical stability, high wear resistance, high stuffing filling performance and other advantages. The polypropylene/polybutylene alloy can improve the fluidity of the material, simultaneously ensure that the dispersibility of the filler in the whole resin system is better, can simultaneously meet the requirements of high fluidity and high rigidity while keeping higher toughness, has low formula cost, and has wider application in the fields of household appliances and automobiles.
For example, patent No. CN03142003.6 discloses a high-fluidity nano talcum powder modified polypropylene composite material and a preparation method thereof, the high-fluidity nano talcum powder modified polypropylene composite material is mainly prepared by blending and extruding polypropylene resin, graft modified polypropylene resin, a rubber toughening agent, a coupling agent and nano talcum powder through a screw extruder set, wherein the size of the nano talcum powder is 30-120 nm, and the impact strength and the elongation at break of the composite material are obviously improved compared with those of a polypropylene composite material taking an inorganic material as a filler. The preparation method is simple and easy to implement. However, the melt index of the polypropylene composite material obtained by the method only reaches 8-10g/10min, and the modulus is only 1800-2100MPa, so that the requirements of large-scale thin-wall products on high fluidity and high rigidity are far not met.
Disclosure of Invention
In order to solve the problems of poor flowability, dispersibility, rigidity and the like of the polypropylene material under excellent impact toughness, the invention provides an alloy composite material with high flowability and high rigidity and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the alloy composite material with high flowability and high rigidity consists of polypropylene resin 60-80 wt%, polybutene resin 10-20 wt%, compatilizer 0.5-3.0 wt%, toughening agent 5-15 wt%, inorganic powder 10-30 wt% and assistant 1-5 wt%.
Further, the polypropylene resin includes one or more of homo-PP resin and co-PP resin.
Further, the polybutene resin includes one or more of isotactic polybutene, syndiotactic polybutene and atactic polybutene.
Further, the compatilizer comprises a PP/PB crosslinking grafting compatilizer.
Further, the PP/PB crosslinking grafting compatilizer comprises an initiator, and the initiator comprises one or more of benzoyl peroxide and dicumyl peroxide.
Further, the toughening agent comprises one or more of POE, high rubber powder, SBS and MBS thermoplastic elastomer mixtures with different impact strengths.
Further, the inorganic powder comprises one or more compound fillers of calcium carbonate, talcum powder, barium sulfate, mica and wollastonite.
Furthermore, the particle size of the filler is 1500-.
Further, the auxiliary agent comprises a lubricant, and the lubricant comprises one or more of stearate and polyethylene wax.
A preparation method of a high-fluidity and high-rigidity alloy composite material comprises the following steps:
preparing a compatilizer:
adding polypropylene resin, polybutylene resin, a compatilizer, a toughening agent, inorganic powder and an auxiliary agent into a high-speed mixer, and mixing for 2-5 min;
and adding the blended material into an extruder, melting, plasticizing, extruding the strips from a die head, cooling, drying, and granulating to obtain the alloy composite material.
Further, the steps for preparing the compatilizer are as follows,
s1: adding PP, PB and xylene solvent into a reactor, slowly stirring and heating to 180-200 ℃;
s2: adding an initiator into the reactor to carry out crosslinking grafting reaction until the raw materials are completely dissolved;
s3: after the raw materials are completely dissolved, reacting at constant temperature of 100-150 ℃ for 0.5-1h to obtain light yellow sticky colloidal liquid;
s4: putting the sticky colloidal liquid obtained in the step S3 into an oven to be dried for 1-2h to obtain a PP/PB crosslinking grafting compatilizer;
further, the mass ratio of PP, PB and xylene solvent is 6-8:2-4: 20.
Further, the mass percent of the initiator is 0.5-2.5%.
Further, the initiator is added into the reactor at least three times, and the time interval of each addition is 45-60 min.
The invention provides a high-fluidity and high-rigidity alloy composite material, which comprises the following raw materials, by weight, 60-80% of polypropylene resin, 10-20% of polybutylene resin, 0.5-3.0% of compatilizer, 5-15% of flexibilizer, 10-30% of inorganic powder and 1-5% of auxiliary agent, so that on the premise of keeping excellent comprehensive mechanical properties, the inorganic powder is well dispersed in a base material, and meanwhile, the fluidity of the material is improved; by adopting the PP/PB cross-linking grafting compatilizer, the compatilizer has the same chain segment with the blend, so that the compatilizer has an emulsifying effect at a PP and PB phase interface, improves the compatibility of a base material polypropylene/polybutylene alloy system, ensures that the polypropylene/polybutylene alloy material has high fluidity, high dispersibility and high rigidity on the premise of excellent impact toughness, realizes the injection molding of large parts on a general injection molding machine, and can be widely applied to multiple fields of household appliances, automobiles and the like.
Drawings
FIG. 1 is a flow chart of a method of making an alloy composite;
FIG. 2 is a flow chart of a method for preparing a compatibilizer in an alloy composite.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments.
The alloy composite material with high flowability and high rigidity consists of polypropylene resin 60-80 wt%, polybutene resin 10-20 wt%, compatilizer 0.5-3.0 wt%, toughening agent 5-15 wt%, inorganic powder 10-30 wt% and assistant 1-5 wt%.
The polypropylene resin comprises one or more of homopolymerized PP resin and copolymerized PP resin, the polypropylene is mainly divided into homopolymerized PP and copolymerized PP according to the difference of PP molecular structures, the homopolymerized PP is completely polymerized by propylene monomers, and the copolymerized PP is mainly polymerized by the propylene monomers and copolymerized with other monomers. The copolymerized PP has excellent impact strength, remarkable tensile strength and better fluidity. According to the performance of the polypropylene composite material, polypropylene resin is selected as homopolymerized PP.
The polybutene resin includes one or more of isotactic polybutene, syndiotactic polybutene and atactic polybutene, and the 1-polybutene is one kind of semi-crystalline thermoplastic polyolefin resin with excellent mechanical performance and three different structures of isotactic, syndiotactic and atactic based on the spatial arrangement of ethylene side group along the main chain.
The compatilizer comprises a PP/PB cross-linked grafting mixture, and the PP/PB cross-linked grafting mixture is subjected to cross-linked grafting reaction by using an initiator, wherein the initiator comprises one or more of benzoyl peroxide and dicumyl peroxide; the compatilizer can play a role in reducing the energy of a two-phase interface, promoting phase dispersion, improving the cohesive force of the phase interface and stabilizing the morphological structure in the reaction of two polymers, thereby improving the performance of the polymer blend, and preferably selecting a thermoplastic elastomer with high mechanical property or mixing two thermoplastic elastomers.
The toughening agent comprises one or more of POE, high rubber powder, SBS and MBS thermoplastic elastomer mixtures with different impact strengths.
The inorganic powder comprises one or more compound fillers of calcium carbonate, talcum powder, barium sulfate, mica and wollastonite, the particle size of the inorganic filler is not the finer, the better, the smaller the particle size, the more difficult uniform dispersion is, the particle size of the filler is between 1500-2500 meshes, the rigidity and the heat resistance of the PP resin can be improved, and the cost can be reduced.
The auxiliary agent comprises a lubricant, wherein the lubricant comprises one or more compounds of stearate and polyethylene wax, and the lubricant can improve the flow property of the polymer, improve the surface smoothness of the modified polypropylene, reduce the energy consumption of equipment and contribute to the uniform dispersion of the flame retardant and the filler in the resin.
Example one
As shown in FIG. 1, a method for preparing a high-fluidity and high-rigidity alloy composite material,
s1: the preparation of the compatilizer is carried out,
s11: adding PP, PB and xylene solvent into a reactor, slowly stirring and heating to 180-200 ℃;
PP is homopolymerized polypropylene, PB is n-butene, the two materials are all general brands, dimethylbenzene is analytically pure, PP: PB: the mass ratio of the dimethylbenzene to the dimethylbenzene is 6:4: 20; the stirring speed is 150-200 r/min;
s12: adding an initiator into the reactor to carry out crosslinking grafting reaction until the raw materials are completely dissolved;
respectively adding 0.5-2.5% of initiator (benzoyl peroxide/dicumyl peroxide) 1h, 2h and 3h after the reaction starts to perform cross-linking grafting reaction;
s13: after the raw materials are completely dissolved, reacting at constant temperature of 100-150 ℃ for 0.5-1h to obtain light yellow sticky colloidal liquid;
after the granules are completely dissolved, keeping the whole system at the constant temperature of 120 ℃ for 1h to finally obtain light yellow sticky colloidal liquid;
s14: drying the sticky colloidal liquid obtained in the step S13 in an oven at 100 ℃ for 2h to obtain a PP/PB crosslinking grafting compatilizer;
s2: the preparation of the alloy composite material is carried out,
adding 60.5% of PP resin, 27.0% of PB resin, 0.0% of compatilizer, 2.0% of flexibilizer, 10.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotating speed of 500r/min for mixing for 3min, then granulating through a double-screw extruder, namely, after melting and plasticizing, extruding strips from a die head, and cooling, drying and granulating at the extrusion processing temperature of 180 ℃ to obtain an alloy composite material;
s3: performance testing of the alloy composite material:
the alloy composite material is placed in an injection molding machine at 160-205 ℃ to be subjected to injection molding to form tensile, bending and impact sample strips, the dimensions of the sample strips are shown in the following table, and the sample strips are placed in an environment with the temperature (23 +/-2) DEG C and the humidity (50 +/-10)% for 88 h.
Tensile bar size:
| length (mm) | Width (mm) | Thickness (mm) |
| 150±2 | 10±0.2 | 4±0.2 |
Bending spline size:
| length (mm) | Width (mm) | Thickness (mm) |
| 80±2 | 10±0.2 | 4±0.2 |
Impact spline size:
| length (mm) | Width (mm) | Thickness (mm) | Gap residual width (mm) |
| 80±2 | 10±0.2 | 4±0.2 | 8±0.2 |
The sample strip is subjected to performance test according to the national standard, and the tensile strength of the alloy composite material is 20.4 MPa; the bending strength is 34.8 MPa; flexural modulus 2310.1 MPa; notched impact 5.3KJ/m2(ii) a Melt index 40.2g/10 min.
Example two
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: adding 80.0% of PP resin, 7.0% of PB resin, 0.0% of compatilizer, 2.0% of flexibilizer, 10.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotating speed of 500r/min for mixing for 3min, then granulating through a double-screw extruder, namely, melting, plasticizing, extruding strips from a die head, cooling, drying and granulating at the extrusion processing temperature of 180 ℃, and thus obtaining the alloy composite material.
Performing performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain that the tensile strength of the alloy composite material is 23.2 MPa; the bending strength is 29.1 MPa; flexural modulus 2210.1 MPa; notched impact 7.6KJ/m2(ii) a Melt index 25.6g/10 min.
EXAMPLE III
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: adding 80.0% of PP resin, 7.0% of PB resin, 0.5% of compatilizer, 2.0% of flexibilizer, 10.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotating speed of 500r/min for mixing for 3min, then granulating through a double-screw extruder, namely, melting, plasticizing, extruding strips from a die head, cooling, drying and granulating at the extrusion processing temperature of 180 ℃, and thus obtaining the alloy composite material.
Carrying out performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain the alloy composite material with the tensile strength of 30.1 MPa; the bending strength is 38.2 MPa; flexural modulus 2530.1 MPa; notched impact of 10.3KJ/m2(ii) a Melt index 30.5g/10 min.
Example four
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: adding 79.5% of PP resin, 6.5% of PB resin, 1.5% of compatilizer, 2.0% of flexibilizer, 10.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotating speed of 500r/min, mixing for 3min, then granulating through a double-screw extruder, namely, melting, plasticizing, extruding strips from a die head, cooling, drying and granulating at the extrusion processing temperature of 180 ℃, and thus obtaining the alloy composite material.
The performance of the prepared alloy composite material is tested according to the mode of the first embodiment to obtain the alloy composite materialUntil the tensile strength is 35.2 MPa; the bending strength is 45.2 MPa; flexural modulus 3012.0 MPa; notched impact 13.2KJ/m2(ii) a Melt index 50.6g/10 min.
EXAMPLE five
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: adding 78.5% of PP resin, 6.0% of PB resin, 3.0% of compatilizer, 2.0% of flexibilizer, 10.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotation speed of 500r/min for mixing for 3min, then granulating through a double-screw extruder, namely, melting, plasticizing, extruding strips from a die head, cooling, drying and granulating at the extrusion processing temperature of 180 ℃, and thus obtaining the alloy composite material.
Performing performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain that the tensile strength of the alloy composite material is 31.0 MPa; the bending strength is 37.6 MPa; flexural modulus 2610.1 MPa; notched impact of 9.4KJ/m2(ii) a Melt index 35.2g/10 min.
EXAMPLE six
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: adding 66.0% of PP resin, 10.0% of PB resin, 1.5% of compatilizer, 2.0% of toughening agent, 20.0% of inorganic powder and 0.5% of auxiliary agent into a high-speed mixer with the rotating speed of 500r/min for mixing for 3min, then granulating through a double-screw extruder, namely, melting, plasticizing, extruding strips from a die head, cooling, drying and granulating at the extrusion processing temperature of 180 ℃, and thus obtaining the alloy composite material.
Carrying out performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain the alloy composite material with the tensile strength of 32.1 MPa; the bending strength is 43.2 MPa; flexural modulus 4031.2 MPa; notched impact of 9.8KJ/m2(ii) a Melt index 45.0g/10 min.
EXAMPLE seven
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: 60.0% of PP resin, 6.0% of PB resin, 1.5% of compatilizer, 2.0% of toughening agent, 30.0% of inorganic powder and 0.5% of auxiliary agent are added into a high-speed mixer with the rotating speed of 500r/min to be mixed for 3min, then granulation is carried out through a double-screw extruder, namely, after melting and plasticizing, strips are extruded from a die head, the extrusion processing temperature is 180 ℃, and the alloy composite material is obtained through cooling, drying and grain cutting.
Carrying out performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain the alloy composite material with the tensile strength of 30.1 MPa; the bending strength is 40.3 MPa; flexural modulus 4510.1 MPa; notched impact 8.6KJ/m2(ii) a Melt index 40.5g/10 min.
Example eight
The difference between the present embodiment and the first embodiment is that S2 is used to prepare an alloy composite material: 60.0% of PP resin, 5.0% of PB resin, 1.5% of compatilizer, 3.0% of toughening agent, 30.0% of inorganic powder and 0.5% of auxiliary agent are added into a high-speed mixer with the rotating speed of 500r/min to be mixed for 3min, then granulation is carried out through a double-screw extruder, namely, after melting and plasticizing, strips are extruded from a die head, the extrusion processing temperature is 180 ℃, and the alloy composite material is obtained through cooling, drying and grain cutting.
Carrying out performance test on the prepared alloy composite material according to the mode of the first embodiment to obtain that the tensile strength of the alloy composite material is 28.3 MPa; the bending strength is 39.6 MPa; flexural modulus 4412.3 MPa; notched impact of 10.2KJ/m2(ii) a Melt index 36.2g/10 min.
It can be seen from the first and second examples that the tensile strength and impact strength are improved with the increase of the ratio of the PB resin, but the flexural strength, flexural modulus and melt index are reduced; compared with the second embodiment and the third embodiment, the addition of the compatilizer can obviously improve the mechanical property of the PP/PB alloy material, and the fluidity is also increased.
It can be seen from the third, fourth and fifth examples that, with the increase of the compatibilizer, the mechanical properties of the PP/PB alloy material are increased and then decreased, and the optimal addition ratio is 1.5%, because the compatibilizer can reduce the energy of the two-phase interface, promote the phase dispersion, improve the cohesive force of the phase interface, and stabilize the morphological structure, thereby improving the properties of the polymer. However, as the content of the compatilizer increases, the compatilizer is used as a third component to hinder crystallization of the compatilizer and reduce crystallinity, so that the mechanical property of the blended alloy is reduced.
It can be seen from the fourth, sixth and seventh examples that the mechanical properties of the PP/PB alloy are reduced to some extent with the increase of the addition amount of the inorganic powder, but the reduction is not obvious, and compared with a formula system without the addition of the compatibilizer, the fluidity, rigidity and toughness of the material are all significantly improved, which indicates that the addition of the compatibilizer can improve the dispersibility of the inorganic powder in the base material.
It can be seen from the seventh and eighth embodiments that, as the addition amount of the toughening agent increases, the toughness of the material is improved to some extent, and the flow property and the mechanical property are only slightly reduced, but the reduction range is acceptable, and the requirements can still be met.
Therefore, the seventh embodiment can obtain the PP/PB alloy composite material with high fluidity and high rigidity.
According to the invention, the PP/PB cross-linked graft mixture is used as the compatilizer, so that the compatibility of a base material polypropylene/polybutylene alloy system is improved, the polypropylene/polybutylene alloy material is ensured to have high fluidity, high dispersibility and high rigidity on the premise of excellent impact toughness, a large-sized workpiece is injected on a general injection molding machine, and the PP/PB cross-linked graft mixture can be widely applied to multiple fields of household appliances, automobiles and the like.
The above description is only a preferred embodiment of the present invention, but the design concept of the present invention is not limited thereto, and any insubstantial modifications made by using the design concept should fall within the scope of infringing on the protection scope of the present invention.
Claims (14)
1. A high-fluidity and high-rigidity alloy composite material is characterized in that: the raw materials comprise, by weight, 60-80% of polypropylene resin, 10-20% of polybutylene resin, 0.5-3.0% of compatilizer, 5-15% of flexibilizer, 10-30% of inorganic powder and 1-5% of auxiliary agent.
2. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the polypropylene resin comprises one or more of homopolymerized PP resin and copolymerized PP resin.
3. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the polybutene resin includes one or more of isotactic polybutene, syndiotactic polybutene and atactic polybutene.
4. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the compatilizer comprises a PP/PB crosslinking grafting compatilizer.
5. The high-fluidity, high-rigidity alloy composite material according to claim 4, wherein: the PP/PB crosslinking grafting compatilizer comprises an initiator, and the initiator comprises one or more of benzoyl peroxide and dicumyl peroxide.
6. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the toughening agent comprises one or more of POE, high rubber powder, SBS and MBS thermoplastic elastomer mixtures with different impact strengths.
7. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the inorganic powder comprises one or more compound fillers of calcium carbonate, talcum powder, barium sulfate, mica and wollastonite.
8. The high-flow, high-rigidity alloy composite according to claim 7, characterized in that: the particle size of the filler is 1500-2500 meshes.
9. The high-fluidity, high-rigidity alloy composite material according to claim 1, wherein: the auxiliary agent comprises a lubricant, and the lubricant comprises one or more compounds of stearate and polyethylene wax.
10. A preparation method of a high-fluidity and high-rigidity alloy composite material is characterized by comprising the following steps: the alloy composite according to any one of claims 1 to 9, prepared by the following process:
preparing a compatilizer;
adding polypropylene resin, polybutylene resin, a compatilizer, a toughening agent, inorganic powder and an auxiliary agent into a high-speed mixer, and mixing for 2-5 min;
and adding the blended material into an extruder, melting, plasticizing, extruding the strips from a die head, cooling, drying, and granulating to obtain the alloy composite material.
11. The method of preparing a high-fluidity, high-rigidity alloy composite according to claim 10, wherein: the steps for preparing the compatibilizer are as follows,
s1: adding PP, PB and xylene solvent into a reactor, slowly stirring and heating to 180-200 ℃;
s2: adding an initiator into the reactor to carry out crosslinking grafting reaction until the raw materials are completely dissolved;
s3: after the raw materials are completely dissolved, reacting at constant temperature of 100-150 ℃ for 0.5-1h to obtain light yellow sticky colloidal liquid;
s4: and (5) putting the sticky colloidal liquid obtained in the step S3 into an oven to be dried for 1-2h, so as to obtain a PP/PB cross-linked grafting mixture.
12. The method of preparing a high-fluidity, high-rigidity alloy composite according to claim 11, wherein: the mass ratio of the PP, PB and xylene solvents is 3-4:1-2: 10.
13. The method of preparing a high-fluidity, high-rigidity alloy composite according to claim 11, wherein: the mass percentage of the initiator is 0.5-2.5%.
14. A method for preparing a high-fluidity, high-rigidity alloy composite material according to claim 11 or 13, wherein: the initiator is added into the reactor at least three times, and the time interval of each addition is 45-60 min.
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| CN113549268A (en) * | 2021-07-19 | 2021-10-26 | 山东京博石油化工有限公司 | Foamed polypropylene material and preparation method thereof |
| CN115322490A (en) * | 2022-08-23 | 2022-11-11 | 广东圆融新材料有限公司 | Extrusion-grade low-dielectric-constant polypropylene material and preparation method thereof |
| CN115678164A (en) * | 2022-11-23 | 2023-02-03 | 江苏新合益机械有限公司 | High-strength alloy composite material and preparation method thereof |
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Application publication date: 20200512 |