CN114395195A - Low-odor polypropylene material with good appearance and preparation method thereof - Google Patents
Low-odor polypropylene material with good appearance and preparation method thereof Download PDFInfo
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- CN114395195A CN114395195A CN202210131292.7A CN202210131292A CN114395195A CN 114395195 A CN114395195 A CN 114395195A CN 202210131292 A CN202210131292 A CN 202210131292A CN 114395195 A CN114395195 A CN 114395195A
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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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- 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
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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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 of polypropylene material automobile parts, the dispersibility of the filler in the components is high, so that the appearance of poor surfaces is avoided, and the odor of the product is reduced compared with the existing product; the product has low cost and high qualification rate. The invention also discloses a preparation method of the low-odor polypropylene material with good appearance and application of the low-odor 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 automobile reserves in China and the rapid development of automobile industry, the demand of the industry for automobile modified plastics is increasing day by day. Polypropylene is widely used because of its good processability, low material density and relatively low cost. However, since polypropylene resins have disadvantages such as poor heat resistance and low toughness, it is necessary to modify them by adding a toughening agent, a filler, and the like.
In the field of modified polypropylene for vehicles, an inorganic filler is generally added as a component to reinforce a polypropylene material, and common inorganic fillers include talc powder, calcium carbonate, mica powder and the like. However, since the fillers mentioned above are present in the form of powder, they are easily dispersed unevenly or aggregated when added directly during the modification of polypropylene. When the filler is agglomerated, on one hand, the mechanical property of the product is unstable, and on the other hand, appearance defects such as pits and pits of the product can be caused, and at present, in addition to basic performance and processing requirements, each main engine plant also puts higher and higher requirements on the appearance of the automobile. Based on this trend, the existing products have been unable to meet such requirements.
CN102391572A discloses a high-toughness calcium carbonate filled polypropylene composite material and a preparation method thereof, wherein the aim of rigidity and toughness enhancement is achieved by adding ultrafine calcium carbonate, but in order to increase the compatibility of calcium carbonate and a polypropylene matrix, a titanate coupling agent with high price is added, so that compared with a talcum powder reinforced material with equivalent filling amount, the cost performance is too low, and industrial mass production cannot be realized. CN104419059A discloses a high-strength and high-toughness polypropylene material and a preparation method thereof, wherein the dispersion uniformity of fillers is increased by adding composite master batches containing mica powder and nano calcium carbonate, but the mica powder used by the material is of a sheet structure, so that the appearance of a finished product has a phenomenon of 'shining' similar to that of a glass fiber reinforced material, and the material is not suitable for automobile appearance parts. In addition, the polypropylene composite material contains more organic components which can generate small molecular substances such as phenol, aldehyde and the like at high temperature, and the small molecular substances have high odor, so that the prepared automobile parts have peculiar smell easily.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide a low-odor polypropylene material with good appearance, and the product has high dispersibility of fillers in the components on the premise that the mechanical properties meet the requirements of most polypropylene material automobile parts, so that the appearance of poor surfaces cannot appear, and the odor of the product is reduced compared with that of the existing product; the product has low cost and high qualification rate, and is suitable for various application ranges.
In order to achieve the purpose, the invention adopts the technical scheme that:
a low-odor polypropylene material with good appearance 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 a dispersing agent and 3-5 parts of a processing aid;
in the components of the high-performance composite master batch, the melt mass flow rate of POE under the load of 2.16kg at 190 ℃ is more than 4g/10 min;
the average grain diameter of the superfine calcium carbonate is 0.5-5 mu m.
The traditional small-particle-size polypropylene reinforcing filler (such as superfine talcum powder and the like) is easy to agglomerate and disperse unevenly in the processing process, so that the mechanical reinforcing effect is unstable, and the product appearance problem is also brought; the superfine calcium carbonate is spherical, and can play double roles of filling reinforcement and heterogeneous nucleation simultaneously compared with other reinforcing fillers or calcium carbonate with conventional particle size, so that the polypropylene resin is induced to generate more fine spherulites, the mechanical property of the product is improved, but agglomeration is easily caused due to too small particle size, and the appearance performance 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 materials, the carrier is naturally polypropylene resin), however, the processing temperature of the matrix resin is generally high, in the preparation process of the master batch, organic substances (usually from processing aids) in the components are often produced into micromolecule substances with extremely strong smell at high temperature, when the master batch is further used for preparing the composite material, the content of the micromolecule substances is increased by times through secondary high-temperature processing, meanwhile, other components of the composite material except the master batch also contain certain organic substances, and finally the smell of the product is larger, while the POE in the high-performance composite master batch is used as a carrier of the superfine calcium carbonate, so that the processing temperature of the composite master batch can be obviously reduced, after the addition of the high-performance composite master batch and the processing aids in the product are further optimized, no processing aid is additionally added into the components of the product, so that the content of the generated small molecular substances is effectively reduced, and the odor of the whole product is correspondingly reduced.
Preferably, the POE is at least one of an ethylene-butene copolymer and an ethylene-octene copolymer.
Preferably, 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 10-50 g/10min, and the melt flow rate is tested according to ASTM D1238-2010 standard.
The inventor tests that the lower the POE melt flow rate in the high-performance composite master batch, the higher the melt viscosity in the preparation process of the master batch, the higher the shear heat generated in the processing process, and the more remarkable the degradation of the polymer and the antioxidant, so that more micromolecular substances such as aldehyde and ketone are generated, and the odor of the high-performance composite master batch and the polypropylene material prepared from the high-performance composite master batch is improved.
Preferably, the ratio of the mass of the polypropylene resin to the mass of 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 increased, so that the rigidity (flexural modulus) of the obtained product can be effectively improved, and meanwhile, the relative content of odor micromolecule substances generated by other components due to high temperature can be relatively reduced, but the toughness (impact strength) of the product is reduced, and the appearance of the product is also influenced to a certain extent. The comprehensive performance of the product obtained by the addition ratio is optimal through the experimental screening of the inventor.
Preferably, the polypropylene resin is at least one of homo-polypropylene resin and co-polypropylene resin, the melt mass flow rate of the polypropylene resin at 230 ℃ and under a load of 2.16kg is 3-60 g/10min, 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 mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid uniformly, and then mixing and granulating to obtain the high-performance composite master batch.
Preferably, the low-odor polypropylene material with good appearance further comprises 0-2 parts of a toughening agent and 0-10 parts of a polyethylene resin.
According to the toughness mechanical requirements of actual products, technicians in the field can add additional contents of polyethylene resin and toughening agent into the components of the product, and the system of matching the polyethylene resin and the toughening agent can effectively improve the toughness of the product.
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 polypropylene material with good appearance further comprises 0-2 parts of toner.
Preferably, the processing aid is at least one of an antioxidant, a weather resisting agent, a light stabilizer and a lubricant.
More preferably, the antioxidant is a mixture of a hindered phenol type antioxidant and a phosphite type antioxidant;
the light stabilizer is a hindered amine light stabilizer;
the lubricant is zinc stearate amine;
the mass ratio of the hindered phenol antioxidant to the phosphite antioxidant to the hindered amine light stabilizer to the zinc stearate is (0.9-1.1): (0.9-1.1): (0.9-1.1): (0.9 to 1.1);
preferably, the dispersant is at least one of Ethylene Bis Stearamide (EBS) and zinc stearate.
The invention also aims to provide a preparation method of the low-odor polypropylene material with good appearance, which comprises the following steps:
and uniformly mixing the components, adding the mixture into a double-screw extruder, carrying out melt extrusion, granulating and drying to obtain the low-odor polypropylene material with good appearance.
The preparation method of the low-odor polypropylene material with good appearance has simple operation steps and can realize industrial scale production.
Preferably, the temperature setting conditions of the temperature zone of the twin-screw extruder during melt extrusion are as follows: the temperature of the first zone is 100-120 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 210-230 ℃, the temperature of the fourth zone is 210-230 ℃, the temperature of the fifth zone is 210-230 ℃, the temperature of the sixth zone is 210-230 ℃, the temperature of the seventh zone is 210-230 ℃, the temperature of the eighth zone is 210-230 ℃, and the temperature of the ninth zone is 210-230 ℃;
preferably, the rotating speed of a main machine of the double-screw extruder is 250-600 rpm; the length-diameter ratio of the double-screw extruder is 40: 1.
the invention further aims to provide application of the low-odor polypropylene material with good appearance in preparing automobile parts.
The low-odor polypropylene material with good appearance has good appearance, excellent mechanical property, strong controllability, high qualification rate and low odor, and is particularly 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 a low-odor polypropylene material with good appearance, and the product meets the requirements of most polypropylene material automobile parts on the premise of mechanical properties (the flexural modulus reaches over 1800MPa, the notched impact strength of a cantilever beam reaches 15KJ/m2Above, it can be adjusted according to the requirements of practical use), the dispersibility of the filler in the component is high, so that the surface appearance is not poor, and simultaneously, compared with the prior artThe odor of the existing product is reduced; the product has low cost and high qualification rate. The invention also provides a preparation method of the low-odor polypropylene material with good appearance and application of the low-odor polypropylene material in preparation of automobile parts.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments involved in the practice of the present invention are, unless otherwise specified, common reagents and instruments.
Examples 1 to 12
The low-odor good-appearance polypropylene material and the preparation method thereof have the following components shown in table 1.
The preparation method of the low-odor polypropylene material with good appearance comprises the following steps:
and (3) 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 be uniform, adding the mixture into a double-screw extruder to be subjected to melt extrusion, granulating and drying to obtain the low-odor polypropylene material with good appearance.
The temperature setting conditions of the temperature zone of the double-screw extruder during melt extrusion are as follows: the temperature of a first area is 120 ℃, the temperature of a second area is 190 ℃, the temperature of a third area is 210 ℃, the temperature of a fourth area is 210 ℃, the temperature of a fifth area is 210 ℃, the temperature of a sixth area is 230 ℃, the temperature of a seventh area is 230 ℃, the temperature of an eighth area is 230 ℃, and the temperature of a ninth area is 230 ℃;
the rotating speed of a main machine of the double-screw extruder is 350 rpm; the length-diameter ratio of the double-screw extruder is 40: 1.
the components used in the examples were as follows:
the polypropylene resin 1 is a copolymerized polypropylene resin, and is an EP548RQ model product produced by medium sand petrochemical industry, and the melt mass flow rate of the polypropylene resin is 28g/10 min;
the polypropylene resin 2 is homopolymerized polypropylene resin, a 1100N type product produced by Shenhuaning coal, and the melt mass flow rate of the polypropylene resin is 12g/10 min;
the toughening agent is a POEENGAGE 7447 model product produced by the Dow company, and the melt mass flow rate of the toughening agent is 4.5g/10 min;
the polyethylene is HDPE DMDA8008 produced by the petrifaction of the Mount-mountain fruits;
the toner is a commercial black seed;
the high-performance composite master batch 1 is self-made, and the difference between the high-performance composite master batches 2-6 and the high-performance composite master batch 1 is only that the component proportion is different;
the preparation method of the high-performance composite master batch 2-4 comprises the following steps: mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid in a high-speed mixer for 3min, and then putting the mixture into an internal mixer for mixing and granulation to obtain the high-performance composite master batch;
wherein POE1 is POE ENGAGE 8137 product produced by Dow corporation, and the melt flow rate of the ethylene-octene copolymer is 13g/10min at 190 deg.C under 2.16kg load;
POE2 is POE ENGAGE 7447 type product produced by Dow corporation, ethylene-butylene copolymer, and has melt flow rate of 4.5g/10min at 190 deg.C under 2.16kg load;
the superfine calcium carbonate 1 is a product produced in Europe and has an average particle size of 2.5 mu m after particle size screening;
the superfine calcium carbonate 2 is a product produced in Europe and has an average particle size of 5 mu m after particle size screening;
the superfine calcium carbonate 3 is a product produced in Europe and has an average grain diameter of 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 ester antioxidant;
the light stabilizer is a commercially available hindered amine light stabilizer;
the lubricant is commercially available zinc stearate amine;
the mass ratio of the hindered phenol antioxidant to the phosphite antioxidant to the hindered amine light stabilizer to the zinc stearate is as follows: m (hindered phenol antioxidant: phosphite antioxidant: hindered amine light stabilizer: zinc stearate) 1:1:1: 1;
the commercially available starting materials used in the examples were all of the same kind.
TABLE 1
TABLE 2
Comparative example 1
The comparative example is different from example 1 only in that POE1 in the high-performance composite master batch 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 mother particle is replaced with 20 parts of ultrafine calcium carbonate 1 and 5 parts of POE1 in the preparation raw material.
Comparative example 3
The comparative example differs from example 1 only in that the 25 parts of high performance composite masterbatch were replaced with 20 parts of commercially available 3000 mesh talc and 5 parts of POE 1.
Comparative example 4
The comparative example is different from example 1 only in that the ultrafine calcium carbonate 1 in the preparation raw material in the high-performance composite master batch is replaced by calcium carbonate having an average particle size of 150nm, which is manufactured by Keynes nanomaterial Co.
Comparative example 5
The comparative example is different from example 1 only in that the ultrafine calcium carbonate 1 in the preparation raw material in the high-performance composite mother particle is replaced with calcium carbonate having an average particle size of 15 μm manufactured by omega.
Comparative example 6
The comparative example differs from example 1 only in that POE1 was replaced with POE ENGAGE model 7467 from Dow with a melt flow rate of 1.2g/10min at 190 ℃ under a load of 2.16 kg.
Comparative examples 7 to 10
Comparative examples 7-10 differ from example 1 only in component selection as shown in tables 1 and 2.
The raw materials for the components for the comparative example were the same commercial species as those for each example, except for the specific descriptions.
Effect example 1
The products obtained in each example and comparative example are tested for flexural modulus, notched izod impact strength, appearance performance, percent of pass and odor grade:
(1) flexural modulus test: testing the flexural modulus and the flexural speed of the material by adopting ISO178-2010, wherein the flexural modulus is 2 mm/min;
(2) testing the notch impact strength of the cantilever beam: the impact strength of a cantilever notch of the material is tested by adopting ISO180-2000, and the impact pendulum capacity of an A-type notch is 5.5J;
(3) appearance performance: the products obtained in each example and comparative example are injection-molded into 100 × 100 plane square boards with uniform thickness, the surface condition of the square boards is subjected to amplification observation and scanning statistics, and then grading is carried out;
the grade is 1: the front and back surfaces of the square plate have no defects such as powder spots, pockmarks or pits; and 2, stage: the front and back surfaces of the square plate have a small amount of powder dots, pockmarks or pits and other defects, and the number of the defects is less than or equal to 2; and 3, level: the front surface and the back surface of the square plate have certain defects such as powder spots, pockmarks or pits, and the number of the defects is 3-10; 4, level: the front and back surfaces of the square plate have a large number of defects such as powder dots, pockmarks or pits, and the number of the defects is more than 10;
(4) the percent of pass is: the actual output mass/total material input quantity of a qualified sample is 100%, the qualified sample is a formable sample, and byproducts, excess materials and processing sinking non-forming sample materials are removed;
(5) and (3) testing the odor grade: adopting a popular PV3900 method, wherein the temperature is 80 ℃ and the time is 2 h.
The test results are shown in table 3.
TABLE 3
As can be seen from the table, the low-odor polypropylene material with good appearance prepared by the examples of the invention can also achieve 15KJ/m of notched Izod impact strength under the condition that the flexural modulus reaches above 1800MPa2Meanwhile, according to the requirements of practical application, the rigidity and toughness can be adjusted by regulating and controlling the component proportion, and the usable range is very wide; meanwhile, the appearance grade of the obtained product is less than or equal to 2 grade, no obvious defects such as pits and the like appear on the surface, the appearance is good, and the qualification rate is up to more than 98 percent; the odor grade of the obtained product can reach 4 grades or below, and the comprehensive performance is excellent. From the examples 1 and 8-10, it can be seen that the raw material ratio and the type selection of the high-performance composite master batch in the product components have certain influence on the odor performance of the product, particularly, the odor performance of the product is the lowest when the melt mass flow rate of POE is more than 10g/10min, and the odor performance grade of the product in the comparative example 6 reaches 4.5 grade when the melt mass flow rate of POE is less than 4g/10 min. In contrast, the product of comparative example 1, which adopts the calcium carbonate master batch of the commercial polypropylene resin matrix as the filler, has obviously higher odor performance than the product of each example, while the products of comparative examples 2 and 3, which adopt the ultrafine calcium carbonate or the commercial talcum powder as the filler and do not use the ultrafine calcium carbonate or the commercial talcum powder as the master batch for further processing, have the defects of uneven filler agglomeration, poor appearance, more surface pockmarks and the like, and simultaneously lead to lower product yield; the calcium carbonate particle size of the master batch raw material in the product obtained in the comparative example 4 is smaller,the obtained product has serious agglomeration phenomenon, the appearance performance of the product is insufficient, and when the particle size is too large, the mechanical property of the obtained comparative example 5 is insufficient.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The low-odor polypropylene material with good appearance 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 a dispersing agent and 3-5 parts of a processing aid;
in the components of the high-performance composite master batch, the melt mass flow rate of POE under the load of 2.16kg at 190 ℃ is more than 4g/10 min;
the average grain diameter of the superfine calcium carbonate is 0.5-5 mu m.
2. The low-odor polypropylene material with good appearance of claim 1, wherein the POE in the components of the high-performance composite master batch has a melt mass flow rate of 10-50 g/10min at 190 ℃ under a load of 2.16 kg.
3. The low-odor polypropylene material with good appearance according to claim 1, wherein the mass ratio of the polypropylene resin to the high-performance composite master batch is (7:3) - (7.5: 2.5).
4. The low-odor and good-appearance polypropylene material according to claim 1, wherein the polypropylene resin is at least one of a homo-polypropylene resin and a co-polypropylene resin.
5. The low-odor polypropylene material with good appearance as claimed in claim 1, wherein the preparation method of the high-performance composite master batch comprises the following steps: and mixing POE, superfine calcium carbonate, a dispersing agent and a processing aid uniformly, and then mixing and granulating to obtain the high-performance composite master batch.
6. The low-odor good-appearance polypropylene material as claimed in claim 1, wherein the low-odor good-appearance polypropylene material further comprises 0-2 parts of a toughening agent and 0-10 parts of a polyethylene resin.
7. The low odor, good appearance polypropylene material of claim 1 wherein the processing aid is at least one of an antioxidant, a weathering agent, a light stabilizer, a lubricant; the dispersant is at least one of EBS and zinc stearate.
8. The method for preparing the low-odor good-appearance polypropylene material as claimed in any one of claims 1 to 7, comprising the steps of:
and uniformly mixing the components, adding the mixture into a double-screw extruder, carrying out melt extrusion, granulating and drying to obtain the low-odor polypropylene material with good appearance.
9. The method for preparing a low-odor polypropylene material with good appearance according to claim 8, wherein the temperature setting conditions of the temperature zone of the twin-screw extruder during melt extrusion are as follows: the temperature of the first zone is 100-120 ℃, the temperature of the second zone is 190-210 ℃, the temperature of the third zone is 210-230 ℃, the temperature of the fourth zone is 210-230 ℃, the temperature of the fifth zone is 210-230 ℃, the temperature of the sixth zone is 210-230 ℃, the temperature of the seventh zone is 210-230 ℃, the temperature of the eighth zone is 210-230 ℃, and the temperature of the ninth zone is 210-230 ℃;
the rotating speed of a main machine of the double-screw extruder is 250-600 rpm; the length-diameter ratio of the double-screw extruder is 40: 1.
10. use of the low-odor and good-appearance polypropylene material as defined in any one of claims 1 to 7 for the production of automobile parts.
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| CN111892758A (en) * | 2020-07-07 | 2020-11-06 | 广西夏阳环保科技有限公司 | Nano calcium carbonate plastic master batch and preparation method thereof |
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