CN111849068B - Polypropylene composition and preparation method thereof - Google Patents

Polypropylene composition and preparation method thereof Download PDF

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Publication number
CN111849068B
CN111849068B CN201910359954.4A CN201910359954A CN111849068B CN 111849068 B CN111849068 B CN 111849068B CN 201910359954 A CN201910359954 A CN 201910359954A CN 111849068 B CN111849068 B CN 111849068B
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polypropylene
parts
polypropylene composition
composition
odor
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CN111849068A (en
Inventor
雷亮
叶南飚
黄险波
吴亦建
苏娟霞
彭莉
孙刚
吴国峰
杨波
罗忠富
彭忠泉
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Kingfa Science and Technology Co Ltd
Shanghai Kingfa Science and Technology Co Ltd
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Kingfa Science and Technology Co Ltd
Shanghai Kingfa Science and Technology Co Ltd
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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
    • C08L23/12—Polypropene
    • 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
    • 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
    • C08K2201/006—Additives being defined by their surface area
    • 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
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Abstract

The invention discloses a polypropylene composition, which comprises the following components in parts by weight: 63-99 parts of polypropylene resin; 1-5 parts of nano tubular filler; the polypropylene composition has a silicon content of 0.1-2wt% and a magnesium content of 0.1-1.5 wt%. The preparation method comprises the steps of uniformly mixing the components, adding the mixture into a double-screw extruder, carrying out melt mixing at the screw rotating speed of 350-450 rpm and the temperature of 170-220 ℃, and carrying out extrusion granulation to obtain the composite material. The invention reduces the odor of the composition by adding the nano tubular filler into the polypropylene composition.

Description

Polypropylene composition and preparation method thereof
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a polypropylene composition and a preparation method thereof.
Background
Polypropylene (PP) has the advantages of low density, easy processing, excellent mechanical properties, etc., and has been widely used in the fields of automobile industry, home appliances and machinery. For the automotive industry, polypropylene is mainly used for interior and exterior parts of automobiles, such as instrument panels, door panels, pillars and the like, and exterior parts such as bumpers, fenders, deflectors and the like. With the increasing concern about the quality of air in a vehicle, people have higher and higher requirements on the smell in the vehicle. Therefore, the odor of the polypropylene material for automobile interior needs to be reduced.
In order to reduce the odor of polypropylene materials, the main means at present are: selecting raw materials with weaker smell, adding a smell adsorbent, vacuumizing, baking at a later stage and the like. Wherein the odor adsorbent comprises chemical adsorption and physical adsorption. Chemisorption of molecules such as zinc ricinoleate to sequester aldehydes and ketones to reduce odor; physical adsorption such as porous filler mainly comprises diatomite, zeolite, activated carbon, porous silica, porous calcium phosphate, molecular sieve and activated alumina. But the chemical adsorption can only adsorb polar small molecules, and the adsorption effect of most physical adsorbents is not ideal. Although the mode of vacuumizing and post-baking can remove the odorous micromolecules, a large amount of energy consumption is generated, and the requirement of energy conservation is not favorably realized.
The present study surprisingly shows that the addition of a nanotubular filler to a polypropylene composition can effectively reduce the odor of the composition.
Disclosure of Invention
The invention aims to provide a high-performance and low-odor polypropylene composition.
Another object of the present invention is to provide a process for the preparation of the above polypropylene composition.
The invention is realized by the following technical scheme:
a polypropylene composition comprises the following components in parts by weight:
63-99 parts of polypropylene resin;
1-5 parts of nano tubular filler;
in the polypropylene composition, the silicon content is 0.1-2wt%, and the magnesium content is 0.1-1.5 wt%.
Preferably, the composition comprises the following components in parts by weight:
63-99 parts of polypropylene resin;
2-4 parts of nano tubular filler;
in the polypropylene composition, the silicon content is 0.3-1wt%, and the magnesium content is 0.3-0.7 wt%.
The invention researches and discovers that the odor of the composition can be reduced only when the amount of the nano tubular filler is 1-5 parts. When the added nano tubular filler is too small, the odor of the composition is not obviously improved, and when the added nano tubular filler is too much, the viscosity of the material is increased, so that the odor generated in the processing process is more in small molecules, the odor is enhanced, the filler is difficult to disperse due to too much filler, and the odor is not easy to improve.
The silicon and the magnesium in the composition are both derived from the nano tubular filler, and when the silicon content in the composition exceeds 2wt% and the magnesium content in the composition exceeds 1.5wt%, the nano tubular filler is not easy to disperse in the composition, and the odor of the composition is not obviously improved; when the content of silicon in the composition is less than 0.1wt% and the content of magnesium in the composition is less than 0.1wt%, the nano tubular filler is low in water adsorption content, and the odor of the composition is not obviously improved due to less odor small molecules brought by moisture gasification in the processing process.
The nano tubular filler is selected from at least one of nano halloysite, nano sepiolite and nano attapulgite, and the nano sepiolite is preferred. Because the specific surface area of nano-sepiolite is relatively large and it is easily dispersed in the composition.
The specific surface area of the nano tubular filler is 300-700 m2(ii)/g, preferably of 450-550 m2/g。
When the specific surface area of the added nano-tube-shaped filler is smaller, the adsorbed odor micromolecules are fewer, and the odor of the composition is not obviously improved; when the specific surface area of the added nano-tube-shaped filler is larger, the nano-tube-shaped filler is difficult to disperse, and the odor of the composition is not obviously improved.
The polypropylene resin is selected from copolymerized polypropylene or homopolymerized polypropylene resin, the melt mass flow rate of the polypropylene resin is 1-100 g/10min, the test standard is ASTM D1238, and the test conditions are 230 ℃ and 2.16 Kg. When the melt mass flow rate is less than 1g/10min, the material has poor flowability and is not beneficial to processing; when the melt mass flow rate is more than 100g/10min, the small molecular weight part of the material is more, which is not beneficial to eliminating the odor.
The polypropylene composition also comprises 0-30 parts of toughening agent by weight, wherein the toughening agent is selected from one of ethylene-propylene copolymer, ethylene-butylene copolymer, ethylene-octylene copolymer and styrene copolymer elastomer, and the density of the toughening agent is 0.85-0.9 g/cm3The melt mass flow rate is 0.3-30 g/min, the test standard is ASTM D1238, the test conditions are 190 ℃ and 2.16 Kg.
The polypropylene composition also comprises an auxiliary agent, wherein the auxiliary agent comprises one or two of an antioxidant or a light stabilizer.
The preparation method of the polypropylene composition comprises the following steps:
the polypropylene resin, the toughening agent, the nano tubular filler and the auxiliary agent are uniformly mixed and then added into a double-screw extruder, and the mixture is melted and mixed at the screw rotating speed of 350-450 r/min and the temperature of 170-220 ℃, extruded and granulated to obtain the polypropylene composition.
The invention has the following beneficial effects: through research, the nano tubular filler with specific silicon content and magnesium content is added into the polypropylene composition, and when the composition has a certain silicon content and magnesium content, the odor in the composition can be reduced; meanwhile, the nano tubular filler has relatively large specific surface area, and can adsorb odor small molecules, so that the odor of the polypropylene composition is better reduced. In addition, the invention is not required to be implemented by increasing equipment or equipment energy consumption, and is relatively energy-saving.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
The sources of the raw materials used in the present invention are as follows, but are not limited by the following raw materials.
Polypropylene resin a: the homo-polypropylene resin has the melt mass flow rate of 30g/10min, the test standard of ASTM D1238, the test conditions of 190 ℃ and 2.16 Kg;
polypropylene resin B: the copolymerized polypropylene resin has the melt mass flow rate of 1g/10min, the test standard of ASTM D1238, the test conditions of 190 ℃ and 2.16 Kg;
polypropylene resin C: the homo-polypropylene resin has the melt mass flow rate of 100g/10min, the test standard of ASTM D1238, the test conditions of 190 ℃ and 2.16 Kg;
a toughening agent: ethylene-propylene copolymer having a density of 0.85g/cm3The melt mass flow rate is 10g/min, the test standard is ASTM D1238, the test conditions are 190 ℃ and 2.16 Kg;
nanotube-shaped filler a: nano sepiolite with specific surface area of 500 m2/g；
The nano tubular filler B: nanometer halloysite with a specific surface area of 300 m2/g；
Nanotube-shaped filler C: nano concave-convex rod with specific surface area of 700 m2/g；
Diatomite: infilm 300;
an antioxidant A: an antioxidant 1010;
and (3) antioxidant B: an antioxidant 168;
light stabilizer: UV-3808PP 5;
performance test or method criteria:
silicon content: and testing by adopting an inductively coupled plasma atomic emission spectrometry. Weighing 0.2g of sample, placing the sample in a polytetrafluoroethylene digestion tank, respectively adding 10mL of nitric acid and 2mL of hydrogen peroxide, placing the digestion tank in a high-pressure closed microwave digestion instrument after being closed, completely digesting the sample at 220 ℃, cooling the sample to room temperature, completely transferring the digestion solution to a 50mL volumetric flask, washing the inner tank and the inner cover with water for 3 times, merging the washing solution into the volumetric flask, diluting the washing solution to a scale with water, and shaking up. And (4) measuring the test solution by using an inductively coupled plasma atomic emission spectrometer, and determining the silicon content according to a calibration curve.
Weighing 0.2g of sample, placing the sample in a polytetrafluoroethylene digestion tank, respectively adding 10mL of nitric acid and 2mL of hydrogen peroxide, placing the digestion tank in a high-pressure closed microwave digestion instrument after being closed, completely digesting the sample at 220 ℃, cooling the sample to room temperature, completely transferring the digestion solution to a 50mL volumetric flask, washing the inner tank and the inner cover with water for 3 times, merging the washing solution into the volumetric flask, diluting the washing solution to a scale with water, and shaking up. And (4) measuring the test solution by using an inductively coupled plasma atomic emission spectrometer, and determining the content of each element according to a calibration curve.
The content of magnesium: and testing by adopting an inductively coupled plasma atomic emission spectrometry. Weighing 0.2g of sample, placing the sample in a polytetrafluoroethylene digestion tank, respectively adding 10mL of nitric acid and 2mL of hydrogen peroxide, placing the digestion tank in a high-pressure closed microwave digestion instrument after being closed, completely digesting the sample at 220 ℃, cooling the sample to room temperature, completely transferring the digestion solution to a 50mL volumetric flask, washing the inner tank and the inner cover with water for 3 times, merging the washing solution into the volumetric flask, diluting the washing solution to a scale with water, and shaking up. And (4) measuring the test solution by using an inductively coupled plasma atomic emission spectrometer, and determining the magnesium content according to a calibration curve.
Weighing 0.2g of sample, placing the sample in a polytetrafluoroethylene digestion tank, respectively adding 10mL of nitric acid and 2mL of hydrogen peroxide, placing the digestion tank in a high-pressure closed microwave digestion instrument after being closed, completely digesting the sample at 220 ℃, cooling the sample to room temperature, completely transferring the digestion solution to a 50mL volumetric flask, washing the inner tank and the inner cover with water for 3 times, merging the washing solution into the volumetric flask, diluting the washing solution to a scale with water, and shaking up. And (4) measuring the test solution by using an inductively coupled plasma atomic emission spectrometer, and determining the content of each element according to a calibration curve.
And (3) odor test: PV 3900; the results of odor ratings were averaged over 5 odor rater scores and the odor ratings are shown in table 1.
TABLE 1 odor rating PV3900
Scoring Evaluation of
1 Has no odor
2 Odorous but non-interfering odors
3 Has obvious smell and no interference smell
4 Has interfering odor
5 Has strong interfering smell
6 Has intolerable odor
And the test result is the arithmetic mean of the results obtained by the tester, and if the result is not an integer, the nearest half-level is taken as the result.
Examples and comparative examples:
weighing the polypropylene resin, the toughening agent, the nano tubular filler, the antioxidant and the light stabilizer according to the weight parts in the table 2, uniformly mixing the materials, adding the mixture into a double-screw extruder, carrying out melt mixing at the screw rotation speed of 350-450 rpm and the temperature of 170-220 ℃, and carrying out extrusion granulation to obtain the polypropylene composition; the polypropylene compositions were subjected to the odor test, and the results of the respective tests are shown in table 2:
TABLE 2 specific compositions of the respective compositions in examples 1 to 10 and comparative examples 1 to 4 and their test performance results (parts by weight)
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Example 8 Example 9 Example 10 Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4
Polypropylene resin A 77.4 77.4 77.4 77.4 77.4 65 85 95 77.4 77.4 77.4 77.4
Polypropylene resin B 77.4
Polypropylene resin C 77.4
Toughening agent 20 20 20 20 20 30 10 5 20 20 20 20 20 20
Nanotubular Filler A 1 2 3 4 5 3 3 3 10 3
Nanotubular Filler B 3
Nanotube shaped Filler C 3
Diatomite 3
Antioxidant A 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Antioxidant B 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Light stabilizers 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2
Silicon content wt% 0.1 0.5 0.8 1.1 2 0.7 0.8 0.9 0.8 0.8 0.8 0.8 2.2
The content of magnesium is wt% 0.1 0.2 0.5 0.7 1.5 0.5 0.4 0.6 0.5 0.5 0.5 0.1 1.7
Odor grade 3.5 3.5 3.0 3.5 3.5 3.0 3.0 3.0 3.5 3.5 5 4.5 4.0 4.5
As can be seen from the results in table 2, the odor of the composition is reduced after the appropriate amount of nanotubular filler is added. When the tubular nanofiller was added in an amount of 3 parts, the odor of the composition was the lowest. As can be seen from example 3 and comparative example 3, the addition of the nanotubular filler reduced odor better than the addition of the physical adsorbent. The odor of the composition is lowest when the silicon content, the magnesium content, and the specific surface area of the nanotubular filler in the composition are all within the preferred ranges.

Claims (7)

1. The polypropylene composition is characterized by comprising the following components in parts by weight:
63-99 parts of polypropylene resin;
1-5 parts of nano tubular filler;
in the polypropylene composition, the silicon content is 0.1-2wt%, and the magnesium content is 0.1-1.5 wt%;
the nano tubular filler is selected from at least one of nano sepiolite and has the specific surface area of 450-550 m2/g。
2. The polypropylene composition according to claim 1, wherein the composition comprises the following components in parts by weight:
63-99 parts of polypropylene resin;
2-4 parts of nano tubular filler;
in the polypropylene composition, the silicon content is 0.3-1wt%, and the magnesium content is 0.3-0.7 wt%.
3. The polypropylene composition according to claim 1 or 2, wherein the polypropylene resin is selected from a co-polypropylene or a homo-polypropylene resin; the melt mass flow rate of the polypropylene resin is 1-100 g/10min, the test standard is ASTM D1238, and the test conditions are 230 ℃ and 2.16 Kg.
4. The polypropylene composition according to claim 1 or 2, further comprising 0 to 30 parts by weight of a toughening agent selected from one of ethylene-propylene copolymer, ethylene-butene copolymer, ethylene-octene copolymer, styrene copolymer elastomer.
5. The polypropylene copolymer of claim 4, wherein the toughening agent has a density of 0.85 to 0.9 g/cm3, a melt mass flow rate of 0.3 to 30 g/min, ASTM D1238 under test conditions of 190 ℃ and 2.16 Kg.
6. The polypropylene composition according to claim 1 or 2, further comprising 0.2 to 2 parts by weight of an auxiliary agent, wherein the auxiliary agent comprises one or both of an antioxidant and a light stabilizer.
7. Process for the preparation of a polypropylene composition according to any one of claims 1 to 6, comprising the steps of: the polypropylene resin, the toughening agent, the nano tubular filler and the auxiliary agent are uniformly mixed and then added into a double-screw extruder, and the mixture is melted and mixed at the screw rotating speed of 350-450 r/min and the temperature of 170-220 ℃, extruded and granulated to obtain the polypropylene composition.
CN201910359954.4A 2019-04-30 2019-04-30 Polypropylene composition and preparation method thereof Active CN111849068B (en)

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Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101469094B (en) * 2007-12-28 2012-12-05 上海普利特复合材料股份有限公司 Novel low odor polypropylene composite material and preparation thereof
CN105968578A (en) * 2016-06-30 2016-09-28 苏州荣昌复合材料有限公司 Preparation method of low-VOC glass fiber reinforced polypropylene halogen-free flame-retardant composite material
CN107033453A (en) * 2017-03-20 2017-08-11 四川光亚塑胶电子有限公司 A kind of extrusion sheet special-purpose anti-flaming nanometer composite polypropylene material and preparation method thereof
CN108659352A (en) * 2017-03-27 2018-10-16 武汉金发科技有限公司 A kind of polypropylene-nano-attapulgite composite material and preparation method
CN109306117A (en) * 2018-09-06 2019-02-05 江苏圣纳米科技有限公司 Dedicated suppression taste enhancing additive of a kind of micro-foaming polypropylene and preparation method thereof

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