CN114395195B - Low-odor good-appearance polypropylene material and preparation method thereof - Google Patents
Low-odor good-appearance polypropylene material and preparation method thereof Download PDFInfo
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- CN114395195B CN114395195B CN202210131292.7A CN202210131292A CN114395195B CN 114395195 B CN114395195 B CN 114395195B CN 202210131292 A CN202210131292 A CN 202210131292A CN 114395195 B CN114395195 B CN 114395195B
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention discloses a low-odor polypropylene material with good appearance and a preparation method thereof, belonging to the technical field of plastic materials. On the premise that the mechanical properties of the product meet the requirements of most polypropylene material automobile parts, the dispersibility of the filler in the components is high, so that the product does not have poor surface appearance, and meanwhile, compared with the existing product, the odor of the product is reduced; the product has low cost and high qualification rate. The invention also discloses a preparation method of the low-odor good-appearance polypropylene material and application of the low-odor good-appearance polypropylene material in preparation of automobile parts.
Description
Technical Field
The invention relates to the technical field of plastic materials, in particular to a low-odor polypropylene material with good appearance and a preparation method thereof.
Background
With the continuous improvement of the automobile conservation amount in China and the rapid development of the automobile industry, the demand of the industry for the modified plastics for automobiles is increasing. Polypropylene is widely used because of its good processability, low material density and relatively low cost. However, polypropylene resins have disadvantages such as poor heat resistance and low toughness, and therefore, it is necessary to modify them by adding a toughening agent, a filler, or the like.
In the field of modified polypropylene for vehicles, an inorganic filler is generally added as a component to play a role in reinforcing a polypropylene material, and common inorganic fillers include talcum powder, calcium carbonate, mica powder and the like. However, since the fillers exist in the form of powder, the fillers are directly added in the modification process of polypropylene, and the phenomena of uneven dispersion, agglomeration and the like are easy to occur. When the filler is agglomerated, on one hand, the mechanical property of the product is easy to be unstable, and on the other hand, the appearance defects of pits, pits and the like of the finished product are also caused, and at present, all host factories have higher and higher requirements on the aesthetic property of the automobile appearance parts besides basic performance and processing requirements. Based on this trend, existing products must not meet this requirement.
CN102391572a discloses a high-toughness calcium carbonate filled polypropylene composite material and a preparation method thereof, which achieves the purpose of rigidity and toughness enhancement by adding superfine calcium carbonate, but in order to increase the compatibility of calcium carbonate and a polypropylene matrix, a high-price titanate coupling agent is added, so that compared with a talcum powder reinforcing material with equivalent filling amount, the cost performance is too low, and industrial mass production cannot be realized. CN104419059a discloses a polypropylene material with high strength and high toughness and a preparation method thereof, wherein the dispersion uniformity of the filler is increased by adding composite master batch containing mica powder and nano calcium carbonate, but the used mica powder is of a sheet structure, and the appearance of a finished product has a 'brightening' phenomenon similar to that of a glass fiber reinforced material, and is not suitable for automobile appearance parts. In addition, the polypropylene composite material contains a large amount of organic components capable of generating small molecular substances such as phenol, aldehyde and the like at high temperature, and the small molecular substances have high odor and easily cause the prepared automobile part to have odor.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide the low-odor good-appearance polypropylene material, and the product has high dispersibility of the filler in the components on the premise that the mechanical properties meet the requirements of most of polypropylene material automobile parts, so that the poor-surface appearance cannot occur, and meanwhile, compared with the existing product, the odor of the product is reduced; the product has low cost and high qualification rate, and can be suitable for various application ranges.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the low-odor good-appearance polypropylene material comprises the following components in parts by weight:
50-90 parts of polypropylene resin and 12-40 parts of high-performance composite master batch;
the high-performance composite master batch comprises the following components in parts by weight: 15-25 parts of POE, 75-85 parts of superfine calcium carbonate, 1-2 parts of dispersing agent and 3-5 parts of processing aid;
in the components of the high-performance composite master batch, the melt mass flow rate of POE at 190 ℃ under the load of 2.16kg is more than 4g/10min;
the average grain diameter of the superfine calcium carbonate is 0.5-5 mu m.
The traditional polypropylene small-particle-size reinforcing filler (such as superfine talcum powder and the like) is easy to generate agglomeration and uneven dispersion in the processing process, so that not only is the mechanical reinforcing effect unstable, but also the appearance problem of a product is brought, and the superfine calcium carbonate is used as a filler main body, and meanwhile, POE is used as a carrier to form composite master batches, so that the agglomeration phenomenon of the superfine calcium carbonate in polypropylene resin can be effectively inhibited, the compatibility of the superfine calcium carbonate and a polypropylene resin matrix can be improved, and the appearance defect and low qualification rate caused by direct powder addition are avoided; the superfine calcium carbonate is spherical, compared with reinforcing fillers with other shapes or calcium carbonate with conventional particle sizes, the superfine calcium carbonate can play the dual roles of filling reinforcement and heterogeneous nucleation at the same time, and the polypropylene resin is induced to generate more tiny spherulites, so that the mechanical property of the product is improved, but the agglomeration phenomenon is easily caused by the too small particle size, and the appearance property of the product is influenced.
In addition, in order to maintain high compatibility with matrix resin, the matrix resin is often used as a carrier (in polypropylene composite material, the carrier is naturally polypropylene resin), however, the processing temperature of the matrix resin is generally higher, in the preparation process of the matrix resin, the higher temperature often leads organic matters (usually from processing aids) in the components to produce small molecular matters with extremely strong odor, when the matrix is further used for preparing the composite material, the content of the small molecular matters is doubled by secondary high-temperature processing, meanwhile, other components except the matrix of the composite material also contain certain organic matters, and finally, the odor of the product is larger.
Preferably, the POE is at least one of an ethylene-butene copolymer and an ethylene-octene copolymer.
Preferably, among the components of the high performance composite masterbatch, the POE has a melt mass flow rate of 10 to 50g/10min at 190℃under a load of 2.16kg, the melt flow rate being tested according to ASTM D1238-2010.
Through tests, when the POE melt flow rate in the high-performance composite master batch is lower, the melt viscosity in the preparation process of the master batch is higher, the shearing heat generated in the processing process is also higher, and the degradation of the high polymer and the antioxidant is more remarkable, so that more small-molecular substances such as aldehyde, ketone and the like are generated, and the odor of the high-performance composite master batch and the prepared polypropylene material is improved.
Preferably, the mass ratio of the polypropylene resin to the high-performance composite master batch in the components of the low-odor good-appearance polypropylene material is (7:3) - (7.5:2.5).
The content of the high-performance composite master batch is improved, so that the rigidity (flexural modulus) of the obtained product can be effectively improved, and the relative content of odor micromolecular substances generated by other components at high temperature can be relatively reduced, however, the toughness (impact strength) of the product is reduced, and the appearance of the product is influenced to a certain extent. Through experimental screening of the inventor, the comprehensive performance of the product obtained when the additive amount is mixed is optimal.
Preferably, the polypropylene resin is at least one of homo-polypropylene resin and co-polypropylene resin, and the polypropylene resin has a melt mass flow rate of 3-60 g/10min under a load of 2.16kg at 230 ℃, and the melt mass flow rate is tested according to ASTM D1238-2010 standard.
Preferably, the preparation method of the high-performance composite master batch comprises the following steps: and uniformly mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid, and then mixing and granulating to obtain the high-performance composite master batch.
Preferably, the low-odor good-appearance polypropylene material further comprises 0-2 parts of toughening agent and 0-10 parts of polyethylene resin.
According to the toughness mechanical requirement of an actual product, a person skilled in the art can add additional content of polyethylene resin and a toughening agent into the components of the product, and the toughness of the product can be effectively improved by a system combining the polyethylene resin and the toughening agent.
More preferably, the polyethylene is at least one of high density polyethylene, low density polyethylene, linear low density polyethylene;
more preferably, the toughening agent is POE.
Preferably, the low odor and good appearance polypropylene material further comprises 0 to 2 parts of toner.
Preferably, the processing aid is at least one of an antioxidant, a weather-resistant agent, a light stabilizer and a lubricant.
More preferably, the antioxidant is a mixture of hindered phenol type antioxidants and phosphite type antioxidants;
the light stabilizer is a hindered amine light stabilizer;
the lubricant is zinc amine stearate;
the mass ratio of the hindered phenol antioxidant, the phosphite antioxidant, the hindered amine light stabilizer and the zinc stearate is (0.9-1.1): (0.9-1.1): (0.9-1.1): (0.9 to 1.1);
preferably, the dispersing agent is at least one of Ethylene Bis Stearamide (EBS) and zinc stearate.
Another object of the present invention is to provide a method for preparing the low odor and good appearance polypropylene material, comprising the steps of:
and after uniformly mixing the components, adding the components into a double-screw extruder for melt extrusion, granulating and drying to obtain the low-odor good-appearance polypropylene material.
The preparation method of the low-odor and good-appearance polypropylene material has simple operation steps and can realize industrial mass production.
Preferably, the temperature setting conditions of the temperature zone of the twin-screw extruder during melt extrusion are as follows: the first area temperature is 100-120 ℃, the second area temperature is 190-210 ℃, the third area temperature is 210-230 ℃, the fourth area temperature is 210-230 ℃, the fifth area temperature is 210-230 ℃, the sixth area temperature is 210-230 ℃, the seventh area temperature is 210-230 ℃, the eighth area temperature is 210-230 ℃, and the ninth area temperature is 210-230 ℃;
preferably, the rotating speed of a host machine of the double-screw extruder is 250-600 rpm; the aspect ratio of the twin-screw extruder was 40:1.
the invention also aims to provide the application of the low-odor good-appearance polypropylene material in preparing automobile parts.
The low-odor good-appearance polypropylene material disclosed by the invention has the advantages of good appearance, excellent mechanical property, strong controllability, high qualification rate and low odor, and is especially suitable for preparing parts with higher comprehensive performance requirements such as automobile door panels, instrument panels and the like.
The invention has the beneficial effects that the invention provides the low-odor good-appearance polypropylene material, and the product has the flexural modulus reaching more than 1800MPa and the cantilever notched impact strength reaching 15KJ/m on the premise that the mechanical property meets the requirements of most of polypropylene material automobile parts 2 The composition can be adjusted according to the requirements of practical application), and the dispersibility of the filler in the composition is high, so that the appearance of poor surface is avoided, and meanwhile, compared with the prior product, the odor of the composition is reduced; the product has low cost and high qualification rate. The invention also provides a preparation method of the low-odor good-appearance polypropylene material and application of the low-odor good-appearance polypropylene material in preparation of automobile parts.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and the object of the present invention is to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents and instruments involved in the practice of the present invention are common reagents and instruments unless otherwise specified.
Examples 1 to 12
In one embodiment of the low odor and good appearance polypropylene material and the preparation method thereof, the components of the low odor and good appearance polypropylene material are shown in table 1.
The preparation method of the low-odor good-appearance polypropylene material comprises the following steps:
and mixing the polypropylene resin, the high-performance composite master batch, the toughening agent, the polyethylene and the toner in a high-speed mixer for 3min to uniformity, adding the mixture into a double-screw extruder for melt extrusion, granulating and drying to obtain the low-odor and good-appearance polypropylene material.
The temperature setting conditions of the temperature zone of the double-screw extruder during melt extrusion are as follows: first region temperature 120 ℃, second region temperature 190 ℃, third region temperature 210 ℃, fourth region temperature 210 ℃, fifth region temperature 210 ℃, sixth region temperature 230 ℃, seventh region temperature 230 ℃, eighth region temperature 230 ℃, and ninth region temperature 230 ℃;
the rotating speed of a main machine of the double-screw extruder is 350rpm; the aspect ratio of the twin-screw extruder was 40:1.
the components used in each example are as follows:
the polypropylene resin 1 is a copolymerized polypropylene resin, and is produced in a medium sand petrochemical manner and is manufactured in an EP548RQ model, wherein the melt mass flow rate of the polypropylene resin is 28g/10min;
the polypropylene resin 2 is a homopolymerized polypropylene resin, and is a 1100N model product produced by Shenhuaining coal, and the melt mass flow rate of the polypropylene resin is 12g/10min;
the toughening agent is POENGAGE 7447 type product produced by the Dow company, and the melt mass flow rate of the toughening agent is 4.5g/10min;
the polyethylene is HDPE DMDA8008 produced by the petrifaction of Dushan mountain;
the toner is commercially available black seeds;
the high-performance composite master batch 1 is self-made, and the high-performance composite master batches 2-6 and the high-performance composite master batch 1 only have different component proportions;
the preparation method of the high-performance composite master batch 2-4 comprises the following steps of: mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid in a high-speed mixer for 3min uniformly, and then putting the mixture into an internal mixer for mixing and granulating to obtain the high-performance composite master batch;
wherein POE1 is POE ENGAGE 8137 type product produced by Dow company, and the ethylene-octene copolymer has a melt flow rate of 13g/10min under the load of 2.16kg at 190 ℃;
POE2 is POE ENGAGE 7447 model product manufactured by Dow company, ethylene-butene copolymer with melt flow rate of 4.5g/10min under 2.16kg load at 190 ℃;
superfine calcium carbonate 1 is produced by omega, and the average grain diameter is 2.5 mu m after grain diameter screening;
superfine calcium carbonate 2 is a product produced by omega, and the average grain diameter is 5 mu m after grain diameter screening;
superfine calcium carbonate 3 is produced by omega, and the average grain diameter is 0.5 mu m after grain diameter screening;
the dispersing agent is a mixture of commercial EBS and zinc stearate in a ratio of 1:1;
the processing aid comprises an antioxidant, a light stabilizer and a lubricant;
the antioxidant is a commercially available hindered phenol antioxidant and a commercially available phosphite antioxidant;
the light stabilizer is a commercially available hindered amine light stabilizer;
the lubricant is commercially available zinc amine stearate;
the mass ratio of the hindered phenol antioxidant, the phosphite antioxidant, the hindered amine light stabilizer and the zinc stearate is as follows: m (hindered phenol antioxidant: phosphite antioxidant: hindered amine light stabilizer: zinc stearate) =1:1:1:1;
the commercial materials used in each example were all of the same type.
TABLE 1
TABLE 2
Comparative example 1
The only difference between this comparative example and example 1 is that POE1 in the high performance composite masterbatch was replaced with polypropylene resin 1.
Comparative example 2
The comparative example differs from example 1 only in that the 25 parts of the high-performance composite master batch were replaced with 20 parts of ultrafine calcium carbonate 1 and 5 parts of POE1 in the preparation raw materials.
Comparative example 3
The only difference between this comparative example and example 1 is that the 25 parts of high performance composite masterbatch was replaced with 20 parts of commercially available 3000 mesh talc and 5 parts of POE1.
Comparative example 4
The comparative example differs from example 1 only in that the ultrafine calcium carbonate 1 in the preparation raw material in the high-performance composite master batch was replaced with calcium carbonate having an average particle diameter of 150nm produced by Kanden nanomaterial Co.
Comparative example 5
The comparative example differs from example 1 only in that the ultrafine calcium carbonate 1 in the preparation raw material in the high-performance composite master batch was replaced with calcium carbonate having an average particle diameter of 15 μm produced by omega company.
Comparative example 6
The only difference between this comparative example and example 1 is that the POE1 was replaced with a model POE ENGAGE 7467 manufactured by Dow, and the melt flow rate was 1.2g/10min at 190℃under a load of 2.16 kg.
Comparative examples 7 to 10
Comparative examples 7 to 10 differ from example 1 only in the choice of components, as shown in tables 1 and 2.
The component materials used in the comparative examples and those used in the examples were all of the same commercially available variety, except for the specific descriptions.
Effect example 1
The products obtained in each example and comparative example were tested for flexural modulus, notched Izod impact strength, appearance, yield and odor rating:
(1) Flexural modulus test: the flexural modulus of the material was tested using ISO178-2010, flexural rate 2mm/min;
(2) Testing the notch impact strength of the cantilever beam: testing the impact strength of a cantilever beam notch of a material by adopting ISO180-2000, wherein the impact pendulum capacity of the A-type notch is 5.5J;
(3) Appearance performance: the products obtained in each example and comparative example are injection molded into a plane square plate with uniform thickness of 100 x 100, the surface condition of the square plate is subjected to amplification observation and scanning statistics, and then the square plate is rated;
grade 1: the front and back surfaces of the square plate have no defects such as powder spots, pits or pits; 2 stages: the front and back surfaces of the square plate have a small number of defects such as powder spots, pits or pits, and the number of the defects is less than or equal to 2;3 stages: the front and back surfaces of the square plate have certain defects such as powder points, pits or pits, and the number of the defects is 3-10; 4 stages: the front and back surfaces of the square plate have a large number of defects such as powder spots, pits or pits, and the number of the defects is more than 10;
(4) Yield is as follows: the actual output mass/total input amount of materials of the qualified sample is 100%, the qualified sample is a formable sample, and byproducts, residual materials and non-formable sample materials for processing are removed;
(5) Odor rating test: the temperature is 80 ℃ and the time is 2 hours by adopting the popular PV3900 method.
The test results are shown in Table 3.
TABLE 3 Table 3
As can be seen from the table, the low-odor good-appearance polypropylene material prepared by the embodiments of the invention can also reach 15KJ in the case that the flexural modulus reaches more than 1800MPa/m 2 The rigidity and the toughness can be regulated and controlled by the component proportion according to the requirements of practical application, and the application range is extremely wide; meanwhile, the appearance grade of the obtained product is less than or equal to 2, obvious pits and other defects do not appear on the surface, the appearance is good, and the qualification rate is as high as more than 98 percent; the odor grade of the obtained product can reach 4 grade or below, and the comprehensive performance is excellent. As is clear from examples 1 and 8-10, the selection of the raw material ratio and the kind of the high-performance composite master batch in the product component has a certain influence on the odor of the product, especially the melt mass flow rate of POE, when the melt mass flow rate of POE is more than 10g/10min, the odor of the product is the lowest, and when the melt mass flow rate of POE is less than 4g/10min, the odor grade of the product of comparative example 6 reaches 4.5. In contrast, the comparative example 1 using the commercial polypropylene resin matrix as the filler has significantly higher odor than the products of each example, while the comparative examples 2 and 3 using the superfine calcium carbonate or commercial talc powder as the filler and not further processing the same as the master batch have the defects of poor appearance, more surface pits and the like due to uneven aggregation of the filler, and also have lower qualification rate; the particle size of the calcium carbonate particles of the master batch raw material in the product obtained in the comparative example 4 is smaller, the agglomeration phenomenon of the obtained product is serious, the appearance performance of the product is insufficient, and when the particle size is too large, the mechanical performance of the obtained product in the comparative example 5 is insufficient.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The low-odor good-appearance polypropylene material is characterized by comprising the following components in parts by weight:
50-90 parts of polypropylene resin and 12-40 parts of high-performance composite master batch;
the high-performance composite master batch comprises the following components in parts by weight: 15-25 parts of POE, 75-85 parts of superfine calcium carbonate, 1-2 parts of dispersing agent and 3-5 parts of processing aid;
in the components of the high-performance composite master batch, the melt mass flow rate of POE at 190 ℃ under the load of 2.16kg is more than 4g/10min;
the average grain diameter of the superfine calcium carbonate is 0.5-5 mu m.
2. The low odor, good appearance polypropylene material of claim 1, wherein the melt mass flow rate of POE in the composition of said high performance composite masterbatch is 10 to 50g/10min at 190 ℃ under a load of 2.16 kg.
3. The low odor, good appearance polypropylene material of claim 1, wherein the mass ratio of polypropylene resin to high performance composite masterbatch is from (7:3) to (7.5:2.5).
4. The low odor, good appearance polypropylene material of claim 1, wherein said polypropylene resin is at least one of a homo-polypropylene resin and a co-polypropylene resin.
5. The low odor, good appearance polypropylene material of claim 1, wherein the high performance composite masterbatch is prepared by the steps of: and uniformly mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid, and then mixing and granulating to obtain the high-performance composite master batch.
6. The low odor, good appearance polypropylene material of claim 1, further comprising 0 to 2 parts of a toughening agent and 0 to 10 parts of a polyethylene resin.
7. The low odor, good appearance polypropylene material of claim 1, wherein said processing aid is at least one of an antioxidant, a weathering agent, a light stabilizer, a lubricant; the dispersing agent is at least one of EBS and zinc stearate.
8. The method for producing a low-odor and good-appearance polypropylene material according to any one of claims 1 to 7, comprising the steps of:
and after uniformly mixing the components, adding the components into a double-screw extruder for melt extrusion, granulating and drying to obtain the low-odor good-appearance polypropylene material.
9. The method for producing a low-odor and good-appearance polypropylene material according to claim 8, wherein the twin-screw extruder is provided with the following temperature setting conditions in the melt extrusion: the first area temperature is 100-120 ℃, the second area temperature is 190-210 ℃, the third area temperature is 210-230 ℃, the fourth area temperature is 210-230 ℃, the fifth area temperature is 210-230 ℃, the sixth area temperature is 210-230 ℃, the seventh area temperature is 210-230 ℃, the eighth area temperature is 210-230 ℃, and the ninth area temperature is 210-230 ℃;
the rotating speed of a host machine of the double-screw extruder is 250-600 rpm; the aspect ratio of the twin-screw extruder was 40:1.
10. use of a low odor, good appearance polypropylene material as defined in any one of claims 1 to 7 for the manufacture of automotive parts.
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