CN107955270B - Polypropylene nano composite material and preparation method thereof - Google Patents
Polypropylene nano composite material and preparation method thereof Download PDFInfo
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/14—Copolymers of propene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
- C08J2423/12—Polypropene
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a polypropylene nano composite material and a preparation method thereof. The composite material is mainly prepared from the following components in parts by mass: 40-80 parts of polypropylene, 5-15 parts of toughening agent, 0.2-0.5 part of antioxidant, 0.3-0.8 part of lubricant and 20-65 parts of nano reinforced master batch. The polypropylene composite material prepared by the invention has good comprehensive performance and high cost performance, wherein the melt flow rate is more than 25g/10min (230 ℃ and 2.16kg), and the impact strength of a simple beam notch at 23 ℃ is more than 25KJ/m2The flexural modulus is more than 1500 MPa. The composite material is particularly suitable for injection molding production of large-scale inner and outer ornaments of automobile (including new energy automobiles) instrument boards, door panels, bumpers and the like.
Description
Technical Field
The invention relates to a novel polypropylene nano composite material and a preparation method thereof, belonging to the field of high polymer materials.
Background
Polypropylene, a general-purpose plastic, has many excellent properties, but has disadvantages of low mechanical strength, poor heat resistance, large shrinkage deformation, poor creep resistance, and the like. The application, especially as a structural material, is limited and is not a high-performance engineering plastic. Therefore, it is an important research subject to modify and engineer polypropylene.
At present, polypropylene is reinforced and modified, and the method mostly adopts the addition of common grade talcum powder and calcium carbonate. Although the filling modified polypropylene material is widely applied to automobile parts, in order to compensate the great reduction of the impact resistance caused by adding the talcum powder and the calcium carbonate, a large amount of toughening agent is required to be added to improve the impact resistance. Thereby increasing the cost.
Disclosure of Invention
The invention mainly aims to provide a novel polypropylene nano composite material. It is particularly suitable for automotive parts.
The technical scheme of the invention is as follows: the polypropylene nano composite material comprises, by mass, 40-80 parts of polypropylene, 5-15 parts of a toughening agent, 0.2-0.5 part of an antioxidant, 0.3-0.8 part of a lubricant and 20-65 parts of nano reinforced master batch;
the polypropylene, preferably the mixture of the homopolymerized polypropylene and the copolymerized polypropylene, has the mixing ratio of 1:4-6, the product is powdery or granular, and the melt flow rate is 10-60g/10min measured under the conditions of 230 ℃ and 2.16 KG.
The toughening agent is one or a mixture of more than two of polyolefin elastomer ethylene-propylene-octene copolymer, styrene-butadiene copolymer and hydrogenated styrene-butadiene-styrene block copolymer, and the mixing proportion is arbitrary; preferably a polyolefin elastomer ethylene-propylene-octene copolymer (POE), designation DF 610.
The antioxidant is preferably a mixture of a phenolic antioxidant 1010 and a phosphate antioxidant 168, and the ratio of the phenolic antioxidant 1010 to the phosphate antioxidant 168 is preferably 1: 2.
The lubricant is one or a mixture of more than two of calcium stearate, fatty acid ester mixture and ethylene bis-stearamide. Fatty acid ester mixtures are preferred, with the product designation TR044 being preferred.
The preparation formula of the nanometer enhanced master batch comprises the following components in parts by mass:
in the formula, the homopolymerized polypropylene is powder, and the melt flow rate is more than 30g/10 min when measured at 230 ℃ under the condition of 2.16 kg;
the nanometer bath powder is produced by bath and mining companies in Susong county of Anhui province, is a silicon-calcium complex, contains 64-65% of chemical elements of silicon (Si), calcium (Ca), magnesium (Mg) and oxygen (O), has the total sum of the three elements of the other elements of Si, Ca and Mg of 35-36%, and has the particle size of less than 100 nanometers. The bath powder contains flaky particles in a certain proportion, while the traditional talcum powder particles are rod-shaped structures with a certain length-diameter ratio, and the number of the flaky particles is small. The effect of the polypropylene modified by the bath powder is equivalent to that of the traditional talcum powder, but the elongation at break of the polypropylene modified by the bath powder is higher. The nano-scale bath powder is adopted for modification, so that the impact resistance of the polypropylene can be well maintained, and the addition amount of the toughening agent is greatly reduced, thereby reducing the material cost.
The coupling agent is a silane coupling agent, and the preferred product grade is KH 560.
The dispersing agent is preferably polyethylene wax.
The toughening agent is ethylene-methyl methacrylate copolymer (EMMA), the product mark is preferably WH303, and the MMA monomer content is more than or equal to 18%. (ii) a
The polyolefin surface treating agent is a polyolefin plastic regenerant, produced by Lida science and technology (Fujian) Co., Ltd., and is under the brand LD-301.
The preparation method of the polypropylene nano composite material comprises the following steps:
1) preparing a nano reinforced master batch:
(1) diluting the silane coupling agent by using a diluent (preferably industrial absolute ethyl alcohol) for later use, wherein the dilution times are 9-11 times, namely the ratio of the silane coupling agent to the absolute ethyl alcohol is 1: 9-11.
(2) Pouring the weighed nano bath powder into a kneader to be stirred for 5-10 minutes, spraying the diluted silane coupling agent, and continuously sealing and stirring for 30-45 minutes. And (5) finishing the treatment for standby.
(3) Weighing the powdery homopolymerized polypropylene, pouring the powdery homopolymerized polypropylene into a high-speed stirrer, then adding the polyolefin surface treating agent, stirring for 5-8 minutes, and discharging the material for later use.
(4) And (3) respectively weighing the nano bath powder treated in the step (2), the polypropylene treated in the step (3), the toughening agent and the dispersing agent according to the formula design requirements of the nano enhanced master batch, sequentially pouring into a high-speed stirrer, and stirring for 3-5 minutes.
(5) And (3) feeding the high-speed stirred material into a special double-screw extruder for granulation to obtain the nano reinforced master batch.
2) Preparing a polypropylene nano composite material:
(1) the components are weighed according to the formula proportion, poured into a high-speed stirrer in sequence and stirred for 3-5 minutes.
(2) And (3) feeding the stirred materials into a double-screw extruder for extrusion granulation, controlling the temperature at 120 ℃ and 225 ℃, cooling, mixing, detecting and packaging to obtain the finished product of the polypropylene nano composite material.
Compared with the prior art, the invention has the beneficial effects that:
1) the technical scheme of the invention has the outstanding characteristics that: firstly, performing surface treatment on the nano bath powder; and secondly, performing surface treatment on the polypropylene by adopting a polyolefin plastic regenerant, which utilizes the chemical reaction and polymerization principle, mainly generates a synergistic reaction between a plastic interface and a body, grafts polar functional groups on a polypropylene molecular chain, and simultaneously generates a chain extension reaction, increases the interface polarity and the cohesive energy of the polypropylene plastic while improving the molecular weight, thereby improving the affinity with the nano shower gel powder, and has the functions of synchronously realizing the enhancement and toughening. The nano reinforced master batch is prepared at first, so that the use is more convenient, and the filling and reinforcing effects are better.
2) The ethylene-methyl methacrylate copolymer (EMMA) is a novel copolymer, and is safe and sanitary. The invention adopts EMMA to improve the processing thermal stability and the processing fluidity of the nanometer enhanced master batch product, so that the nanometer powder is more effectively dispersed in the polypropylene resin.
3) The polypropylene nano composite material prepared by the formula and the process is detected by adopting ISO standard, and the performance can reach the following standard requirements:
the polypropylene nano composite material prepared by the invention has outstanding impact strength and bending
Modulus and processing fluidity, and is especially suitable for automobile (including new energy automobile) instrument board and automobile
The door panel and other large interior parts are produced by injection molding, and the performance-price ratio is high.
Detailed Description
The technical solution of the present invention is described in detail below, but the scope of the present invention is not limited to the embodiments.
In the following examples and comparative examples,
the copolymerized polypropylene is produced by petrochemical engineering of Beijing Yanshan, and the product brand is K7726H
The toughening agent is produced by Japan Sumitomo chemistry, and the product brand is WH303
The antioxidant is produced by American Yabao, and the product brands are 1010 and 168
The lubricant is produced by Exon of America, and the product mark is TR044
The homopolymerized polypropylene is produced by Ningxia petrochemical company, and the product brand is NX40S
The nanometer bath powder is produced by bath and mining companies of Nardong county of Anhui province, and is a silicon-calcium complex
The coupling agent is produced by Nanjing eosin, and the product is of the brand number KH560
The dispersing agent is polyethylene wax produced by American Honeywell, and the product brand is AC6
The toughening agent is produced by the Japan Triwell, and the product brand is DF610
The polyolefin surface treating agent is manufactured by Lida science and technology (Fujian) Co.Ltd, and is under the brand LD-301.
The preparation formula of the nanometer enhanced master batch comprises the following components in parts by mass:
in this embodiment, the preparation formula comprises, in parts by mass:
in this embodiment, the preparation method of the nano reinforced masterbatch is as follows:
the silane coupling agent is diluted by absolute ethyl alcohol for later use, and the dilution times are 10 times, namely the ratio of the silane coupling agent to the absolute ethyl alcohol is 1: 10.
(1) Pouring the weighed nano bath powder into a kneader to be stirred for 5 minutes, spraying the diluted silane coupling agent, and continuously sealing and stirring for 30 minutes. And (5) finishing the treatment for standby.
(2) And weighing the powdery homopolymerized polypropylene, pouring the powdery homopolymerized polypropylene into a high-speed stirrer, adding the polyolefin surface treating agent, stirring for 5 minutes, and discharging the material for later use.
(3) And (3) respectively weighing the nano bath powder treated in the step (1), the polypropylene treated in the step (2), the toughening agent and the dispersing agent according to the formula design requirements of the nano reinforced master batch, sequentially pouring the materials into a high-speed stirrer, and stirring for 4 minutes.
(4) And (3) feeding the high-speed stirred material into a special double-screw extruder for granulation to obtain the nano reinforced master batch.
Example 1:
formulation for implementation
The implementation process comprises the following steps:
1) the components are weighed according to the formula proportion, poured into a high-speed stirrer in sequence and stirred for 4 minutes.
2) And (3) feeding the stirred materials into a double-screw extruder for extrusion granulation, cooling, mixing, detecting and packaging to obtain the product of the polypropylene nano composite material. Wherein the length-diameter ratio of the double-screw extruder is 40: 1, the temperature of the twin-screw is set to 120 ℃, 170 ℃, 180 ℃, 200 ℃, 210 ℃, and the rotating speed of the extruder at 225 ℃ is 200rpm, the temperature of the water tank is 40 ℃, and the rotating speed of the granulator is 600 rpm.
Example 2:
| formulation material | Weight percent (%) |
| Polypropylene copolymer | 51.2 |
| Toughening agent | 8 |
| Antioxidant agent | 0.3 |
| Lubricant agent | 0.5 |
| Nano reinforced master batch | 40 |
| Total up to | 100 |
The implementation process comprises the following steps:
1) the components are weighed according to the formula proportion, poured into a high-speed stirrer in sequence and stirred for 4 minutes.
2) And (3) feeding the stirred materials into a double-screw extruder for extrusion granulation, cooling, mixing, detecting and packaging to obtain the product of the polypropylene nano composite material. Wherein the length-diameter ratio of the double-screw extruder is 40: 1, the temperature of the twin-screw is set to 120 ℃, 170 ℃, 180 ℃, 200 ℃, 210 ℃, and the rotating speed of the extruder at 225 ℃ is 200rpm, the temperature of the water tank is 40 ℃, and the rotating speed of the granulator is 600 rpm.
Example 2:
the implementation process comprises the following steps:
1) the components are weighed according to the formula proportion, poured into a high-speed stirrer in sequence and stirred for 4 minutes.
2) And (3) feeding the stirred materials into a double-screw extruder for extrusion granulation, cooling, mixing, detecting and packaging to obtain the product of the polypropylene nano composite material. Wherein the length-diameter ratio of the double-screw extruder is 40: 1, the temperature of the twin-screw is set to 120 ℃, 170 ℃, 180 ℃, 200 ℃, 210 ℃, and the rotating speed of the extruder at 225 ℃ is 200rpm, the temperature of the water tank is 40 ℃, and the rotating speed of the granulator is 600 rpm.
Comparative example 1
In the comparative example, the dosage of the nano reinforced master batch is 0 part, and other feeding and processing steps are the same as those of the examples 1 to 3.
The samples obtained in examples 1 to 3 and comparative example 1 were subjected to performance tests, and the results were as follows:
as can be seen from the table, in examples 1-3, compared with comparative example 1, the tensile yield strength and flexural modulus are obviously increased along with the increase of the addition amount of the nano reinforcing master batch, which shows that the nano bath powder has good reinforcing effect.
As can be seen from the table above, the impact strength of the simple beam notch is slightly increased in examples 1-3 compared with comparative example 1, which shows that the nano bath powder not only has good reinforcing effect, but also has a certain toughening effect.
As can be seen from the above table, in examples 1-3, compared with comparative example 1, as the addition amount of the nano reinforcing master batch increases, the melt flow rate decreases in sequence, but the decrease of the melt flow rate is small, which indicates that the processing flowability of the polypropylene nanocomposite is good.
As noted above, while the present invention has been shown and described with reference to certain preferred embodiments, it is not to be construed as limited thereto. Various changes in form and details may be made therein within the scope of the appended claims.
Claims (5)
1. A polypropylene nanocomposite characterized by: the composite material is prepared from the following components in parts by mass:
40-80 parts of polypropylene and 5-15 parts of toughening agent
0.2 to 0.5 portion of antioxidant, 0.3 to 0.8 portion of lubricant
20-65 parts of nano enhanced master batch;
the polypropylene is a mixture of homopolymerized polypropylene and copolymerized polypropylene, and the mixing ratio is 1:4-6, the product is powder or granular; the melt flow rate is 10-60g/10min measured at 230 ℃ under the condition of 2.16 KG; the toughening agent is one or a mixture of more than two of polyolefin elastomer ethylene-propylene-octene copolymer, styrene-butadiene copolymer and hydrogenated styrene-butadiene-styrene block copolymer;
the nanometer reinforced master batch is prepared from the following components in parts by mass:
in the formula, the homopolymerized polypropylene is powder, and the melt flow rate is more than 30g/10 min when measured at 230 ℃ under the condition of 2.16 kg; the nano bath powder is a silicon-calcium complex, and the particle size is less than 100 nanometers; the coupling agent is a silane coupling agent; the dispersing agent is polyethylene wax; the toughening agent is an ethylene-methyl methacrylate copolymer; the polyolefin surface treating agent is a polyolefin plastic regenerant, produced by Lida science and technology (Fujian) Co.Ltd, and is under the brand LD-301;
the preparation method of the nano reinforced master batch comprises the following steps:
(1) diluting the silane coupling agent with absolute ethyl alcohol for later use, wherein the dilution multiple is 9-11 times, namely the ratio of the silane coupling agent to the absolute ethyl alcohol is 1: 9-11;
(2) pouring the weighed nano bath powder into a kneader to be stirred for 5-10 minutes, spraying the diluted silane coupling agent, and continuously sealing and stirring for 30-45 minutes; after the treatment, the mixture is ready for use;
(3) pouring the homopolymerized polypropylene into a high-speed stirrer, adding the polyolefin surface treating agent, and stirring for 5-8 minutes to obtain a material for later use;
(4) respectively weighing the nano bath powder treated in the step (2), the polypropylene treated in the step (3), the toughening agent and the dispersing agent according to the formula of the nano enhanced master batch, sequentially pouring the nano bath powder, the polypropylene treated in the step (3), the toughening agent and the dispersing agent into a high-speed stirrer, and then stirring for 3-5 minutes;
(5) and (3) feeding the high-speed stirred material into a special double-screw extruder for granulation to obtain the nano reinforced master batch.
2. The polypropylene nanocomposite according to claim 1, wherein: the antioxidant is a mixture of a phenol antioxidant 1010 and a phosphate antioxidant 168, and the ratio of the phenol antioxidant to the phosphate antioxidant is 1: 2.
3. The polypropylene nanocomposite according to claim 1, wherein: the lubricant is one or more of calcium stearate, fatty acid ester mixture, and ethylene bisstearamide.
4. Use of the polypropylene nanocomposite according to any one of claims 1 to 3 for large interior and exterior automotive trim parts.
5. A process for the preparation of a polypropylene nanocomposite according to any one of claims 1 to 3 comprising the steps of:
1) preparing a nano reinforced master batch:
(1) diluting the silane coupling agent of claim 1 with absolute ethyl alcohol for later use, wherein the dilution ratio is 9-11 times, namely the ratio of the dilution ratio to the absolute ethyl alcohol is 1: 9-11;
(2) pouring the weighed nano bath powder into a kneader to be stirred for 5-10 minutes,
spraying diluted silane coupling agent, and continuously sealing and stirring for 30-45 minutes; after the treatment, the mixture is ready for use;
(3) pouring the powdery homo-polypropylene as defined in claim 1 into a high-speed mixer, adding the polyolefin surface treating agent as defined in claim 1, and then stirring for 5-8 minutes, the material being ready for use;
(4) respectively weighing the nano bath powder treated in the step (2), the polypropylene treated in the step (3), the toughening agent and the dispersing agent according to the formula of the nano enhanced master batch, sequentially pouring the nano bath powder, the polypropylene treated in the step (3), the toughening agent and the dispersing agent into a high-speed stirrer, and then stirring for 3-5 minutes;
(5) feeding the high-speed stirred material into a special double-screw extruder for granulation to obtain nano enhanced master batches;
2) preparing a polypropylene nano composite material:
(1) weighing the components according to the formula proportion of claim 1, pouring the components into a high-speed stirrer in sequence, and stirring for 3-5 minutes;
(2) and (3) feeding the stirred materials into a double-screw extruder for extrusion granulation, controlling the temperature at 120 ℃ and 225 ℃, cooling, mixing, detecting and packaging to obtain the finished product of the polypropylene nano composite material.
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| EP1479716A1 (en) * | 2003-05-22 | 2004-11-24 | Nmc S.A. | High temperature resistant, flexible, low density polypropylene foams |
| CN102516639A (en) * | 2011-11-14 | 2012-06-27 | 奇瑞汽车股份有限公司 | Modified polypropylene composite material and preparation method thereof |
| CN105802168A (en) * | 2016-05-23 | 2016-07-27 | 江西省萍乡市轩品塑胶制品有限公司 | Biodegradable nanometer filling function master batch and preparation method and application thereof |
| CN106046555A (en) * | 2016-07-28 | 2016-10-26 | 宁夏易兴实业有限公司 | Functional polypropylene coating material and preparation method for same |
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| BRPI1010294A2 (en) * | 2009-04-09 | 2016-03-22 | Borealis Ag | thermoplastic polyolefin composition. |
| CN104194146B (en) * | 2014-08-06 | 2016-09-28 | 惠州市沃特新材料有限公司 | Polypropene composition and preparation method thereof |
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|---|---|---|---|---|
| EP1479716A1 (en) * | 2003-05-22 | 2004-11-24 | Nmc S.A. | High temperature resistant, flexible, low density polypropylene foams |
| CN102516639A (en) * | 2011-11-14 | 2012-06-27 | 奇瑞汽车股份有限公司 | Modified polypropylene composite material and preparation method thereof |
| CN105802168A (en) * | 2016-05-23 | 2016-07-27 | 江西省萍乡市轩品塑胶制品有限公司 | Biodegradable nanometer filling function master batch and preparation method and application thereof |
| CN106046555A (en) * | 2016-07-28 | 2016-10-26 | 宁夏易兴实业有限公司 | Functional polypropylene coating material and preparation method for same |
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