CN106854309B - Low-odor modified polypropylene composite material and preparation method thereof - Google Patents
Low-odor modified polypropylene composite material and preparation method thereof Download PDFInfo
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- CN106854309B CN106854309B CN201611173292.4A CN201611173292A CN106854309B CN 106854309 B CN106854309 B CN 106854309B CN 201611173292 A CN201611173292 A CN 201611173292A CN 106854309 B CN106854309 B CN 106854309B
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- 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
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- 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
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- C08L23/12—Polypropene
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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
- C08K2201/00—Specific properties of additives
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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Abstract
The invention belongs to the technical field of polymer composite materials, and particularly relates to a low-odor modified polypropylene composite material and a preparation method thereof. The composite material comprises polypropylene: 35-87 parts; water-absorbent resin: 3-5 parts; inorganic mineral powder: 0-40 parts; a toughening agent: 10-20 parts; processing aid: 0.3-1.0 part; heat stabilizer masterbatch: 0.2-0.8 part; ozone water: 4-6 parts. The invention introduces ozone water, and the ozone can oxidize low molecular active odor substances such as low molecular aldehydes, ketones, amines, benzenes and the like at high temperature, thereby improving the odor of the polypropylene composite material and reducing the VOC content; the invention introduces ozone water solution, the water solution is vaporized at high temperature to generate a large amount of water vapor, and the supercritical state is formed under the melt pressure, so that low molecules in the polypropylene composite material can be further extracted, the odor of the polypropylene composite material is improved, and the VOC content is reduced.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to a low-odor modified polypropylene composite material and a preparation method thereof.
Technical Field
With the improvement of health and environmental awareness of people, the complaints of peculiar smell and low-melting-point volatile harmful substances (VOC) of aldehydes, benzenes and aliphatic hydrocarbons in passenger cars are more and more serious, and 3.15 in the past year, the national quality inspection bureau issues complaints of consumers about the quality of automobile products in the past year, and the quality of air in new cars becomes the first of four major problems of complaints.
The rapid development of polypropylene modification technology makes the application of polypropylene in automobile interior and exterior trim more and more extensive, however, polypropylene resin and products thereof still release Volatile Organic Compounds (VOC) to different degrees to pollute the environment and harm the health of people due to the influence of monomers, catalysts, polymerization processes, degradation and the like in the synthesis process of polypropylene, and are limited in practical use.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of a low-odor modified polypropylene composite material.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a low-odor modified polypropylene composite material comprises the following raw materials in parts by weight:
the polypropylene is at least one of homopolymerized polypropylene and copolymerized polypropylene, and the melt index of the polypropylene under the conditions of the temperature of 230 ℃ and the load of 2.16kg is 3-100g/10 min.
The water-absorbing resin is one or a mixture of more than two of carboxymethylated cellulose, hydroxypropylated cellulose, chitosan and hydroxymethylated starch.
The inorganic mineral powder is at least one of talcum powder, calcium carbonate, glass fiber, whisker and wollastonite.
The toughening agent is an ethylene elastomer or a styrene elastomer.
The processing aid is at least one of low molecular hydrocarbon, metal soap, stearic acid composite ester and amide processing aids.
The heat stabilizer masterbatch is at least one masterbatch selected from hindered phenol, hindered amine and phosphite heat stabilizer.
The ozone water is 0.1-10mg/kg aqueous solution of ozone.
The preparation method of the low-odor modified polypropylene composite material comprises the following steps:
(1) preparing an odor adsorption material:
putting the water-absorbent resin and the ozone water in the formula into a low-temperature mixer, and mixing and stirring for 5-10min at 20-30 ℃ to prepare an odor adsorption material;
(2) preparing a composite material:
uniformly mixing polypropylene, odor adsorption material, inorganic mineral powder, toughening agent and processing aid according to the weight part ratio in the formula, and then mixing the mixture in a ratio of length-diameter ratio of 35-50: 1, melting, mixing and dispersing, adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and performing double-screw extrusion granulation to obtain the low-odor modified polypropylene composite material.
The invention has the beneficial effects that:
1) according to the invention, ozone is introduced to oxidize low-molecular active odor substances such as low-molecular aldehydes, ketones, amines and benzenes at high temperature, so that the odor of the polypropylene composite material can be improved, and the VOC content can be reduced;
2) the invention introduces ozone, decomposes at high temperature to generate oxygen which can escape through a natural exhaust port;
3) the invention introduces ozone water solution, the water solution is vaporized at high temperature to generate a large amount of water vapor, and the supercritical state is formed under the melt pressure, so that low molecules in the polypropylene composite material can be further extracted, the odor of the polypropylene composite material is improved, and the VOC content is reduced.
The specific implementation mode is as follows:
the following examples are given to illustrate the present invention and it is necessary to point out here that the following examples are given only for the purpose of further illustration and are not to be construed as limiting the scope of the invention, which is intended to be covered by the claims and that the invention will be modified and adapted by those skilled in the art in view of the teachings herein.
All compositions of the present invention are currently commercially available products, wherein:
the toughening agent is ethylene elastomer or styrene elastomer, such as Polyethylene (PE), ethylene-octene Polymer (POE), ethylene-propylene-butadiene terpolymer (EPDM), etc.
The processing aid is at least one of low molecular hydrocarbon, metal soap, stearic acid composite ester and amide processing aids. Mainly refers to calcium stearate (Ca-St)2) Ethylene Bis Stearamide (EBS), modified ethylene bis stearamide (TAF), and the like.
The heat stabilizer is at least one selected from hindered phenols, hindered amines and phosphites, wherein the hindered phenols comprises master batches such as 2, 6-tertiary butyl-4-methylphenol, bis (3, 5-tertiary butyl-4-hydroxyphenyl) thioether or tetra [ β - (3, 5-tertiary butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester (1010), the phosphite heat stabilizers comprise tris (2, 4-di-tertiary butyl phenyl) phosphite (168), trioctyl ester, tridecyl ester or tris (dodecyl) ester and tris (hexadecyl) ester, and the hindered amines comprise master batches such as naphthylamine, diphenylamine and p-phenylenediamine.
In the invention, the low-odor modified polypropylene composite material is prepared by the following method:
(1) preparing an odor adsorption material:
putting the water-absorbent resin and the ozone water in the formula into a low-temperature mixer, and mixing and stirring for 5-10min at 20-30 ℃ to prepare an odor adsorption material;
(2) preparing a composite material:
uniformly mixing polypropylene, odor adsorption material, inorganic mineral powder, toughening agent and processing aid according to the weight part ratio in the formula, and then mixing the mixture in a ratio of length-diameter ratio of 35-50: 1, melting, mixing and dispersing, adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and performing double-screw extrusion granulation to obtain the low-odor modified polypropylene composite material.
Formulations and preparation parameters of examples and comparative examples
The following specific examples 1 to 5 were all prepared by the above-mentioned preparation method for producing a low-odor modified polypropylene composite, and will not be described in detail.
Example 1:
in the embodiment, the water-absorbent resin and the ozone water in the formula are put into a low-temperature mixer and mixed and stirred for 5-10min at the temperature of 20-30 ℃ to prepare the odor adsorption material; and then melting, mixing and dispersing the polypropylene, the odor adsorption material, the inorganic mineral powder, the toughening agent and the processing aid in a double-screw extruder with the length-diameter ratio of 50:1, finally adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and extruding and granulating to obtain the product.
Example 2:
in the embodiment, the water-absorbent resin and the ozone water in the formula are put into a low-temperature mixer and mixed and stirred for 5-10min at the temperature of 20-30 ℃ to prepare the odor adsorption material; and then melting, mixing and dispersing the polypropylene, the odor adsorption material, the inorganic mineral powder, the toughening agent and the processing aid in a double-screw extruder with the length-diameter ratio of 35:1, finally adding the heat-stable master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and extruding and granulating to obtain the product.
Example 3:
in the embodiment, the water-absorbent resin and the ozone water in the formula are put into a low-temperature mixer and mixed and stirred for 5-10min at the temperature of 20-30 ℃ to prepare the odor adsorption material; and then melting, mixing and dispersing the polypropylene, the odor adsorption material, the inorganic mineral powder, the toughening agent and the processing aid in a double-screw extruder with the length-diameter ratio of 40:1, finally adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and extruding and granulating to obtain the product.
Example 4:
in the embodiment, the water-absorbent resin and the ozone water in the formula are put into a low-temperature mixer and mixed and stirred for 5-10min at the temperature of 20-30 ℃ to prepare the odor adsorption material; and then melting, mixing and dispersing the polypropylene, the odor adsorption material, the inorganic mineral powder, the toughening agent and the processing aid in a double-screw extruder with the length-diameter ratio of 40:1, finally adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and extruding and granulating to obtain the product.
Example 5:
in the embodiment, the water-absorbent resin and the ozone water in the formula are put into a low-temperature mixer and mixed and stirred for 5-10min at the temperature of 20-30 ℃ to prepare the odor adsorption material; and then melting, mixing and dispersing the polypropylene, the odor adsorption material, the inorganic mineral powder, the toughening agent and the processing aid in a double-screw extruder with the length-diameter ratio of 40:1, finally adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and extruding and granulating to obtain the product.
Comparative example 1:
the comparative example adopts a double-screw extruder with the length-diameter ratio of 40:1, polypropylene, water-absorbent resin, inorganic mineral powder, a toughening agent and a processing aid are melted, mixed and dispersed in the extruder, then heat stabilizer master batches are fed from the side of the double-screw extruder, and are plasticized and extruded for granulation at the temperature of 170 plus 210 ℃ to obtain the product.
Comparative example 2:
the comparative example adopts a double-screw extruder with the length-diameter ratio of 40:1, polypropylene, water-absorbent resin, inorganic mineral powder, a toughening agent and a processing aid are melted, mixed and dispersed in the extruder, then heat stabilizer master batches are fed from the side of the double-screw extruder, and are plasticized and extruded for granulation at the temperature of 170 plus 210 ℃ to obtain the product.
Test results of second, examples and comparative examples
The samples obtained in examples 1 to 5 and comparative examples 1 to 2 were injection-molded into standard test specimens according to a standard process, in which the tensile strength was measured in units of MPa according to ISO 527/2-93; the flexural modulus test standard is ISO178/2-93, unit MPa; the 23 ℃ notched impact strength test standard is ISO179/2-93, unit kJ/m2. The odor evaluation criteria were: level 1: no odor, grade 2: odorous, but non-interfering odor, grade 3: clear odor, but no interfering odor, grade 4: interfering odor, grade 5: strong interfering odor, grade 6: there is an intolerable smell. VOC test Standard TS-BD-003-. The specific physical property indexes are shown in the following table:
table 1: examples and comparative example physical data
As can be seen from the data of examples 1-5 and comparative examples 1-2, the modified polypropylene composite material meets the requirement of automobile host factories on the grade of less than or equal to 3.5 of odor, and simultaneously, the content of TVOC, benzene and aldehyde low-molecular volatiles is greatly reduced.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (7)
1. A low-odor modified polypropylene composite material is characterized in that: the weight parts of the raw materials are as follows:
polypropylene: 35-87 parts;
water-absorbent resin: 3-5 parts;
inorganic mineral powder: 0-40 parts;
a toughening agent: 10-20 parts;
processing aid: 0.3-1.0 part;
heat stabilizer masterbatch: 0.2-0.8 part;
ozone water: 4.0-6.0 parts;
the ozone water is 0.1-10mg/kg aqueous solution of ozone;
the preparation method of the low-odor modified polypropylene composite material comprises the following steps:
(1) preparing an odor adsorption material:
putting the water-absorbent resin and the ozone water in the formula into a low-temperature mixer, and mixing and stirring for 5-10min at 20-30 ℃ to prepare an odor adsorption material;
(2) preparing a composite material:
uniformly mixing polypropylene, odor adsorption material, inorganic mineral powder, toughening agent and processing aid according to the weight part ratio in the formula, and then mixing the mixture in a ratio of length-diameter ratio of 35-50: 1, melting, mixing and dispersing, adding the heat stabilizer master batch from a side feed of the double-screw extruder, plasticizing at the temperature of 170-210 ℃, and performing double-screw extrusion granulation to obtain the low-odor modified polypropylene composite material.
2. The low odor modified polypropylene composite of claim 1, wherein: the polypropylene is at least one of homo-polypropylene and co-polypropylene, and has a melt index of 3-100g/10min at a temperature of 230 ℃ and a load of 2.16 kg.
3. The low odor modified polypropylene composite of claim 1, wherein: the water-absorbing resin is one or a mixture of more than two of carboxymethylated cellulose, hydroxypropylated cellulose, chitosan and hydroxymethylated starch.
4. The low odor modified polypropylene composite of claim 1, wherein: the inorganic mineral powder is at least one of talcum powder, calcium carbonate, glass fiber, whisker and wollastonite.
5. The low odor modified polypropylene composite of claim 1, wherein: the toughening agent is an ethylene elastomer or a styrene elastomer.
6. The low odor modified polypropylene composite of claim 1, wherein: the processing aid is at least one of low molecular hydrocarbon, metal soap, stearic acid composite ester and amide processing aids.
7. The low odor modified polypropylene composite of claim 1, wherein: the heat stabilizer masterbatch is at least one masterbatch selected from hindered phenol, hindered amine and phosphite heat stabilizer.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109081925B (en) * | 2018-07-02 | 2019-05-14 | 苏州旭光聚合物有限公司 | A kind of supercritical fluid green method efficiently removing smell and VOCs in plastics simultaneously |
| CN109608809B (en) * | 2018-12-07 | 2021-05-25 | 广州市聚赛龙工程塑料股份有限公司 | Low-odor polypropylene composite material and preparation method thereof |
| CN112920504A (en) * | 2019-12-05 | 2021-06-08 | 苏州荣昌复合材料有限公司 | Ultralow-odor reinforced polypropylene composite material and preparation method thereof |
| CN115431433A (en) * | 2022-08-11 | 2022-12-06 | 北方华锦化学工业股份有限公司 | Device and process for preparing low-VOC-content ABS resin by using water as supercritical fluid |
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| CN103571054A (en) * | 2013-10-24 | 2014-02-12 | 合肥会通新材料有限公司 | Low VOC polypropylene composite material and preparation and application thereof |
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