CN115386168A - High-strength flame-retardant material for automotive interior panels and preparation method thereof - Google Patents
High-strength flame-retardant material for automotive interior panels and preparation method thereof Download PDFInfo
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- 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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/20—Oxides; Hydroxides
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- C08K2003/2241—Titanium dioxide
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Abstract
The invention relates to the technical field of flame retardant materials, and discloses a high-strength flame retardant material for an automotive trim panel and a preparation method thereof, wherein the high-strength flame retardant material for the automotive trim panel is prepared by melting, extruding and granulating 8-15 mass ratio of polypropylene resin, ethylene propylene diene monomer, flame retardant modified titanium dioxide, an antioxidant and a compatilizer maleic anhydride grafted polypropylene, wherein the mass ratio is (100).
Description
Technical Field
The invention relates to the technical field of flame retardant materials, in particular to a high-strength flame retardant material for an automotive interior panel and a preparation method thereof.
Background
With the rapid development of industrialization and economy, the yield of automobiles rises year by year, people pursue the quality of automobiles more and more, and pay more attention to the quality, environment friendliness and safety performance of automobiles.
At present, polypropylene (PP) materials used for automobile interior panels are mainly prepared by an injection molding process, and Chinese patent CN103707478B discloses a method for preparing automobile door interior panels or interior column materials by micro-foaming, wherein polypropylene raw materials are added into an injection molding machine for heating and melting to obtain the automobile door interior panels.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-strength flame-retardant material for an automotive interior panel and a preparation method thereof, and solves the problems of poor flame-retardant property and general mechanical property of the traditional automotive interior panel.
In order to achieve the aim, the invention discloses a preparation method of a high-strength flame-retardant material for an automotive interior panel, which comprises the following steps:
uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyltrimethoxysilane, reacting, filtering after the reaction is finished, and drying at 55-65 ℃ for 6-10 hours to obtain epoxy modified titanium dioxide;
step two, uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a nitrogen atmosphere, reacting, performing suction filtration after the reaction is finished, washing with ethanol and deionized water, and performing vacuum drying at 50-60 ℃ for 5-8 hours to obtain aldehyde group modified titanium dioxide;
step three, uniformly mixing an organic solvent, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide, reacting, separating after the reaction is finished, and drying at 55-65 ℃ for 6-10 hours to obtain flame retardant modified titanium dioxide;
and step four, uniformly mixing the polypropylene resin, the ethylene propylene diene monomer, the flame retardant modified titanium dioxide, the antioxidant and the compatilizer maleic anhydride grafted polypropylene, performing melt extrusion at 180-215 ℃, granulating and cooling to obtain the high-strength flame-retardant material for the automotive interior panel.
Preferably, the mass ratio of the absolute ethyl alcohol, the deionized water, the nano titanium dioxide and the gamma-glycidoxypropyltrimethoxysilane in the step one is 1500-2500.
Preferably, the temperature of the reaction in the first step is 75-85 ℃, and the reaction time is 2-4h.
Preferably, in the second step, the mass ratio of the N, N-dimethylformamide to the epoxy modified titanium dioxide to the p-hydroxybenzaldehyde is 2000-3500.
Preferably, the reaction temperature in the second step is 75-105 ℃, and the reaction time is 8-15h.
Preferably, the organic solvent in step three comprises one of tetrahydrofuran, N-dimethylformamide, toluene and acetone.
Preferably, the mass ratio of the organic solvent, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the aldehyde group modified titanium dioxide in the third step is 900-1500.
Preferably, the temperature of the reaction in the third step is 0-5 ℃, and the reaction time is 2-6h.
Preferably, in the fourth step, the mass ratio of the polypropylene resin, the ethylene propylene diene monomer, the flame retardant modified titanium dioxide, the antioxidant and the compatilizer maleic anhydride grafted polypropylene is (100-8-15).
Preferably, the antioxidant in the fourth step comprises one of antioxidant 168, antioxidant 1010 and antioxidant 1076.
Preferably, the high-strength flame-retardant material for the automotive interior panel is prepared by the preparation method of the high-strength flame-retardant material for the automotive interior panel.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, gamma-glycidoxypropyltrimethoxysilane is used for modifying nano titanium dioxide, an epoxy functional group is introduced to the surface of the nano titanium dioxide to obtain epoxy modified titanium dioxide, the epoxy on the surface of the epoxy modified titanium dioxide and the hydroxyl on p-hydroxybenzaldehyde are subjected to ring opening reaction, an aldehyde group is introduced to the surface of the titanium dioxide to obtain aldehyde modified titanium dioxide, the aldehyde group on the surface of the aldehyde modified titanium dioxide and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide are subjected to addition reaction to obtain flame retardant modified titanium dioxide, the flame retardant modified titanium dioxide, polypropylene resin, ethylene propylene diene monomer, antioxidant and compatilizer maleic anhydride are grafted with polypropylene, and the high-strength flame retardant material for the automotive interior panel is obtained through melt extrusion and granulation.
2. The nano titanium dioxide used in the invention has excellent antibacterial performance, under the illumination condition, electrons can be excited to a conduction band from a valence band in a water and air system, corresponding holes are generated in the valence band to generate electron-hole pairs, under the action of an electric field, the electrons and the holes are separated and migrate to the surface of the nano titanium dioxide, and the formed superoxide radical reacts with organic matters in bacteria to decompose the bacteria, thereby killing the bacteria, and the prepared high-strength flame retardant material for the automotive trim panel has excellent antibacterial effect after being added into a polypropylene resin matrix. After the nano titanium dioxide is modified, the agglomeration of the nano titanium dioxide is effectively avoided, the nano titanium dioxide has excellent mechanical property, is uniformly dispersed in a polypropylene resin matrix and is combined with ethylene propylene diene monomer to form a uniform mechanical network structure in the matrix, and when an external force is applied, silver stripes can be initiated around a matrix interface phase to absorb the external force, so that the nano titanium dioxide has excellent mechanical property. The flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is introduced to the nano titanium dioxide, acid substances such as phosphoric acid and phosphorous acid can be generated in the combustion process, the formation of a carbon layer on the surface of a polypropylene resin matrix is promoted, heat is prevented from being transferred to the interior of the matrix, the combustion reaction is effectively inhibited, the nano titanium dioxide can be separated out from the interior in the combustion process and attached to the surface of the carbon layer, the strength of the carbon layer is improved, the direct burning of flame is effectively isolated, the flame-resistant time is prolonged, and the prepared high-strength flame-retardant material for the automotive trim panel is excellent in flame retardant property and mechanical property and is a high-strength flame-retardant material.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a high strength flame retardant material for automotive interior panels;
FIG. 2 is a schematic diagram of the synthesis of aldehyde-modified titanium dioxide in accordance with the present invention;
FIG. 3 is a schematic diagram of the synthesis of flame retardant modified titanium dioxide in the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments, and based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without making creative efforts belong to the protection scope of the present invention.
Example 1
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 1500 to 600;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 2000;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 900;
(4) Uniformly mixing the polypropylene resin, ethylene propylene diene monomer rubber, flame retardant modified titanium dioxide, antioxidant 168 and compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 2
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 1800 to 750, reacting at 80 ℃ for 2.5 hours, filtering after the reaction is finished, and drying at 60 ℃ for 8 hours to obtain epoxy modified titanium dioxide;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 2400;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1050;
(4) Uniformly mixing polypropylene resin, ethylene propylene diene monomer, flame retardant modified titanium dioxide, antioxidant 168 and compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 3
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 2100 to 850, reacting at 80 ℃ for 3 hours, filtering after the reaction is finished, and drying at 60 ℃ for 8 hours to obtain epoxy modified titanium dioxide;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 2800;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1200;
(4) Uniformly mixing the polypropylene resin, the ethylene propylene diene monomer rubber, the flame retardant modified titanium dioxide, the antioxidant 168 and the compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 4
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyltrimethoxysilane in a mass ratio of 2300;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 3200;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1400;
(4) Uniformly mixing the polypropylene resin, the ethylene propylene diene monomer rubber, the flame retardant modified titanium dioxide, the antioxidant 168 and the compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 5
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 2500;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 3500;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1500;
(4) Uniformly mixing the polypropylene resin, ethylene propylene diene monomer rubber, flame retardant modified titanium dioxide, antioxidant 168 and compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 6
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 2300;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 3200;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1400;
(4) Uniformly mixing the polypropylene resin, the ethylene propylene diene monomer rubber, the flame retardant modified titanium dioxide, the antioxidant 1010 and the compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Example 7
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 2300;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 3200;
(3) Uniformly mixing N, N-dimethylformamide, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and aldehyde group modified titanium dioxide in a mass ratio of 1400;
(4) Uniformly mixing polypropylene resin, ethylene propylene diene monomer, flame retardant modified titanium dioxide, antioxidant 1076 and compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Comparative example 1
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidyl ether oxypropyl trimethoxy silane in a mass ratio of 2300;
(2) Uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a mass ratio of 3200;
(3) Uniformly mixing polypropylene resin, ethylene propylene diene monomer, aldehyde modified titanium dioxide, an antioxidant 168 and a compatilizer maleic anhydride grafted polypropylene in a mass ratio of 100.
Comparative example 2
The preparation method of the high-strength flame-retardant material for the automotive interior trim panel comprises the following steps:
(1) Uniformly mixing polypropylene resin, ethylene propylene diene monomer, nano titanium dioxide, an antioxidant 168 and a compatilizer maleic anhydride grafted polypropylene according to a mass ratio of 100.
The nano titanium dioxide used in the embodiment and the comparative example is purchased from New Xuancheng Crystal-Rui material Co., ltd, the model is JR05, and the average particle size is 5nm; the polypropylene resin is purchased from Daqing petrochemical company of China petroleum, the model is T30S, and the Melt Flow Index (MFI) is 3.0g/min; the ethylene propylene diene monomer is purchased from Yiyi plastic science and technology Limited company, and the brand is Miao chemical three-well, and the model is 3092; the maleic anhydride-grafted polypropylene was purchased from Shanghai-day-old technical development Co., ltd, model CMG9801.
The automotive interior panels prepared in examples 1 to 5 and comparative examples 1 to 2 were subjected to thermoforming with a high-strength flame retardant material to prepare samples that met the relevant standard tests, and then to a performance test.
(1) And (3) testing mechanical properties: the tensile property is carried out according to GB/T1040.2-2006 test standard, the high-strength flame-retardant material for the automotive interior panel prepared in the examples 1-5 and the comparative examples 1-2 is cut into sample strips with the size of 180mm multiplied by 10mm multiplied by 4mm, the tensile speed is 50mm/min, and a CMT4101 type electronic tensile testing machine is used for testing; notched impact strength was measured according to GB/T1843-2008 test standards, the high-strength flame-retardant material for automobile interior panels prepared in examples 1-5 and comparative examples 1-2 was cut into bars of 80mm × 10mm × 4mm in size, the thickness of the remaining notch was 2mm, and the test was performed using a model XIJ-5 simple beam impact tester, and the test results are shown in Table 1:
TABLE 1 mechanical Property test Table
According to the test results in Table 1, the mechanical properties of the sample strips of examples 1-5 and comparative example 1 are obviously improved compared with the mechanical properties of the sample strips prepared in comparative example 2, the tensile strength of the sample strip of example 5 can reach 20.5MPa, and the notched impact strength of the sample strip of example 4 can reach 24.2kJ/m 2 (ii) a In the comparative example 1, the nano titanium dioxide is modified, so that the agglomeration of the nano titanium dioxide in a matrix is effectively avoided, but the added aldehyde modified titanium dioxide has more amount and has certain influence on the mechanical property; in comparative example 2, the nano titanium dioxide is not modified, and the nano titanium dioxide is easy to agglomerate in the matrix, so that the nano titanium dioxide has a large influence on the mechanical property of the matrix.
(2) And (3) testing the flame retardant property: the high-strength flame-retardant materials for the automotive interior panels prepared in examples 1 to 5 and comparative examples 1 to 2 were subjected to a limiting oxygen index test with reference to a GB/T2406.2-2009 oxygen index method-plastic combustion performance experimental method for flame retardancy, and the test results are shown in table 2:
TABLE 2 flame-retardant Property test Table
Test items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 |
Limiting oxygen index (%) | 28.7 | 29.3 | 29.5 | 30.0 | 30.2 | 26.2 | 24.1 |
According to the test results in table 2, it can be seen that the high-strength flame retardant material for the automotive interior panels obtained by adding the flame retardant modified titanium dioxide in the examples 1-5 has excellent flame retardant performance, the limited oxygen index range is greater than 27%, the flame retardant is not added in the comparative examples 1-2, but the aldehyde modified titanium dioxide is added in the comparative example 1, the nano titanium dioxide is added in the comparative example 2, the flame retardant performance of the matrix is improved to a certain extent, and the flame retardant effect is difficult to achieve by only adding the nano titanium dioxide.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the high-strength flame-retardant material for the automotive interior panel is characterized by comprising the following steps of: the method comprises the following steps:
step one, uniformly mixing absolute ethyl alcohol, deionized water, nano titanium dioxide and gamma-glycidoxypropyltrimethoxysilane, reacting, filtering after the reaction is finished, and drying to obtain epoxy modified titanium dioxide;
step two, uniformly mixing N, N-dimethylformamide, epoxy modified titanium dioxide and p-hydroxybenzaldehyde in a nitrogen atmosphere, reacting, and after the reaction is finished, performing suction filtration, washing and drying to obtain aldehyde group modified titanium dioxide;
step three, uniformly mixing the organic solvent, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the aldehyde group modified titanium dioxide, reacting, separating and drying after the reaction is finished to obtain the flame retardant modified titanium dioxide;
and step four, uniformly mixing the polypropylene resin, the ethylene propylene diene monomer, the flame retardant modified titanium dioxide, the antioxidant and the compatilizer maleic anhydride grafted polypropylene, performing melt extrusion at 180-215 ℃, granulating and cooling to obtain the high-strength flame-retardant material for the automotive interior panel.
2. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the mass ratio of the absolute ethyl alcohol, the deionized water, the nano titanium dioxide and the gamma-glycidyl ether oxygen propyl trimethoxy silane in the first step is 1500-2500.
3. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: in the second step, the mass ratio of the N, N-dimethylformamide to the epoxy modified titanium dioxide to the p-hydroxybenzaldehyde is 2000-3500.
4. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the reaction temperature in the second step is 75-105 ℃, and the reaction time is 8-15h.
5. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the organic solvent in the third step comprises one of tetrahydrofuran, N-dimethylformamide, toluene and acetone.
6. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the mass ratio of the organic solvent, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and the aldehyde group modified titanium dioxide in the third step is 900-1500.
7. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the reaction temperature in the third step is 0-5 ℃, and the reaction time is 2-6h.
8. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: in the fourth step, the mass ratio of the polypropylene resin, the ethylene propylene diene monomer, the flame retardant modified titanium dioxide, the antioxidant and the compatilizer maleic anhydride grafted polypropylene is (100-8-15).
9. The preparation method of the high-strength flame-retardant material for the automotive interior trim panel according to claim 1, characterized in that: the antioxidant in the fourth step comprises one of antioxidant 168, antioxidant 1010 and antioxidant 1076.
10. The high-strength flame-retardant material for the automotive interior panel, which is prepared by the preparation method of the high-strength flame-retardant material for the automotive interior panel according to any one of claims 1 to 9.
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CN115386168B (en) | 2023-02-24 |
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