CN113444317B - Preparation method of highlight flame-retardant polypropylene material - Google Patents
Preparation method of highlight flame-retardant polypropylene material Download PDFInfo
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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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Abstract
The invention discloses a preparation method of a high-gloss flame-retardant polypropylene material, belonging to the technical field of preparation of high-performance high polymer materials. The highlight flame-retardant polypropylene material is prepared by firstly mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 1,3:2, 4-di-p-methyl benzylidene sorbitol, polypropylene grafted maleic anhydride, an antioxidant and polypropylene, and then carrying out melt blending, extrusion and granulation. The polypropylene material prepared by the invention has excellent flame retardance, high glossiness, good mechanical property and strong thermo-oxidative aging resistance, has wide application prospect in the field of electric appliance shells, and has high economic value and social benefit.
Description
Technical Field
The invention belongs to the technical field of preparation of high-performance high polymer materials, and particularly relates to a preparation method of a high-gloss flame-retardant polypropylene material.
Background
Polypropylene is a semi-crystalline type linear high polymer with regular molecular chain structure and crystallinity up to 60%, and is thermoplastic general-purpose plastic with minimum density in the existing synthetic resin. The heat resistance and the corrosion resistance of the polypropylene are good, and the chemical composition and the aggregation structure of the polypropylene ensure that the polypropylene has good mechanical property and insulating property. The excellent performance of polypropylene makes it widely used in appliance manufacturing, packaging and household appliance fields. However, polypropylene is a compound composed of carbon and hydrogen elements, has an oxygen index of 17-18%, is extremely easy to burn, and is accompanied with a molten drop phenomenon during burning, so that fire can easily spread and cause fire. This limits its application to the appliance housing. The addition of flame retardant in polypropylene is a common means for improving the flame retardance of polypropylene at present. However, the conventional flame retardant has high polarity and poor compatibility with polypropylene, and is easy to migrate to the surface of polypropylene in the using process, so that the flame retardant effect of the polypropylene is influenced. In addition, as the living standard of people is improved, the aesthetic consciousness of people is enhanced, and the shell of the electric appliance is required to have excellent glossiness. However, the gloss of ordinary polypropylene is gradually unsatisfactory. When the 1,3:2, 4-di-p-methyl benzylidene sorbitol is used as a nucleating agent of polypropylene, polypropylene spherulite particles are finer and more uniform, and when the size of the spherulite is smaller than the wavelength of visible light, the visible light transmittance and the surface gloss of the material are both obviously improved. Research shows that when polypropylene is crystallized, 2 free hydroxyl groups of 1,3:2, 4-di-p-methyl benzylidene sorbitol are above the melting point of polypropylene, a three-dimensional nano-network structure is formed through hydrogen bonding, the specific surface area is increased, a gel phenomenon is generated, a large number of crystal nuclei are generated, the crystallization speed is increased, and finally the crystallinity and the glossiness of the polypropylene are improved.
Disclosure of Invention
The invention provides a preparation method of a high-gloss flame-retardant polypropylene material, aiming at the problems of easy combustion, poor glossiness and the like of polypropylene. The polypropylene material prepared by the invention has excellent flame retardance, high glossiness, good mechanical property and strong thermo-oxidative aging resistance, has wide application prospect in the field of electric appliance shells, and has high economic value and social benefit.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-gloss flame-retardant polypropylene material is prepared by firstly mixing 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 1,3:2, 4-di-p-methylbenzylidene sorbitol, polypropylene grafted maleic anhydride, an antioxidant and polypropylene, and then carrying out melt blending, extrusion and granulation on the mixture.
The preparation method of the highlight flame-retardant polypropylene material specifically comprises the following steps:
(1) adding 1-2 g of glycidol into 200-500 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 20-60 min, heating to 80-120 ℃, adding 3-12 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously magnetically stirring for reacting for 6-12 h, pouring the reaction solution into a large amount of water, filtering the separated solid, washing and drying to prepare 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol.
(2) 10-20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.05-0.4 part of 1,3:2, 4-di-p-methylbenzylidene sorbitol, 5-10 parts of polypropylene grafted maleic anhydride, 0.5-1 part of antioxidant and 100 parts of polypropylene are mixed for 10-30 min by a high-speed mixer, the initial mixture is subjected to melt blending by a double-screw extruder, the melting temperature is 200-260 ℃, the screw rotating speed is 60-120 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
In the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
Compared with the prior art, the invention has the following advantages:
(1) the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is a halogen-free flame retardant with excellent performance. However, the compatibility of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide with polypropylene is poor, 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is directly added to polypropylene, and after a period of time, the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is easy to migrate to the surface of polypropylene, so that the flame retardance of polypropylene is reduced. The invention grafts glycidol on 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide molecules through chemical reaction, thereby grafting two hydroxyl groups on 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide. Two hydroxyl groups in 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol and two hydroxyl groups of 1,3:2, 4-di-p-methyl benzylidene sorbitol can better promote the 1,3:2, 4-di-p-methyl benzylidene sorbitol to play the role of a nucleating agent through the action of hydrogen bonds, thereby improving the glossiness of polypropylene and reducing the dosage of the 1,3:2, 4-di-p-methyl benzylidene sorbitol.
(2) Under the action of 1,3:2, 4-di-p-methylbenzylidene sorbitol and polypropylene grafted maleic anhydride, migration of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidyl in polypropylene is limited, and the stability of the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidyl in the polypropylene can be obviously improved.
(3) The polypropylene material prepared by the invention has excellent flame retardance, high glossiness, good mechanical property and strong thermo-oxidative aging resistance. Before thermo-oxidative aging, the polypropylene material has a vertical combustion grade of V-1 or V-2, a glossiness of 117.3-126.5%, a tensile strength of 36.5-38.2 MPa, and an impact strength of 10.6-11.9 kJ/m2After thermo-oxidative aging, the polypropylene material has a vertical burning grade of V-1 to V-2, a glossiness of 112.6 to 119.8%, a tensile strength of 29.3 to 34.8 MPa, and an impact strength of 8.4 to 11.1 kJ/m2The method can be widely used for manufacturing shells of electric appliances such as household appliances, outdoor appliances, industrial and mining appliances and the like, and has higher economic value and social benefit.
Detailed Description
The advantages and effects of the highly photo-flammable polypropylene material in this embodiment are further illustrated by the following examples and comparative examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
(1) Adding 1 g of glycidol into 200 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 20 min, heating to 80 ℃, adding 3 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously and magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously and magnetically stirring for reaction for 12 h, pouring the reaction solution into a large amount of water, filtering to separate out solid, washing and drying to prepare the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol.
(2) 10 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.05 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 5 parts of polypropylene grafted maleic anhydride, 0.5 part of antioxidant and 100 parts of polypropylene are mixed for 10 min by a high-speed mixer, the initial mixture is subjected to melt blending by a double-screw extruder, the melting temperature is 200 ℃, the screw rotating speed is 60 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
In the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
Example 2
(1) Adding 1.5 g of glycidol into 350 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 40 min, heating to 100 ℃, adding 8 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously and magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously and magnetically stirring for reaction for 9 h, pouring the reaction solution into a large amount of water, filtering to separate out solid, washing and drying to prepare the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol.
(2) 15 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.2 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 7 parts of polypropylene grafted maleic anhydride, 0.7 part of antioxidant and 100 parts of polypropylene are mixed for 20 min by a high-speed mixer, the initial mixture is subjected to melt blending by a double-screw extruder, the melting temperature is 230 ℃, the screw rotating speed is 90 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
In the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
Example 3
(1) Adding 2 g of glycidol into 500 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 60 min, heating to 120 ℃, adding 12 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously and magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously and magnetically stirring for reaction for 6 h, pouring the reaction solution into a large amount of water, filtering to separate out solid, washing and drying to prepare the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol.
(2) 20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.4 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 10 parts of polypropylene grafted maleic anhydride, 1 part of antioxidant and 100 parts of polypropylene are mixed for 30 min by a high-speed mixer, the initial mixture is subjected to melt blending by a double-screw extruder, the melting temperature is 260 ℃, the rotating speed of a screw is 120 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
In the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
Comparative example 1
Mixing 20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 0.4 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 10 parts of polypropylene grafted maleic anhydride, 1 part of antioxidant and 100 parts of polypropylene for 30 min by using a high-speed mixer, carrying out melt blending on the primary mixed material by using a double-screw extruder, wherein the melting temperature is 260 ℃, the rotating speed of a screw is 120 rpm, and carrying out extrusion, granulation and drying to obtain the highlight flame-retardant polypropylene material.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
In the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
Comparative example 2
(1) Adding 2 g of glycidol into 500 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 60 min, heating to 120 ℃, adding 12 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously and magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously and magnetically stirring for reaction for 6 h, pouring the reaction solution into a large amount of water, filtering to separate out solid, washing and drying to prepare the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol.
(2) 20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.4 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 1 part of antioxidant and 100 parts of polypropylene are mixed for 30 min by a high-speed mixer, the initial mixture is melted and blended by a double-screw extruder, the melting temperature is 260 ℃, the screw rotating speed is 120 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
Comparative example 3
Mixing 20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 0.4 part of 1,3:2, 4-di-p-methyl benzylidene sorbitol, 1 part of antioxidant and 100 parts of polypropylene for 30 min by using a high-speed mixer, carrying out melt blending on the initial mixture by using a double-screw extruder, wherein the melting temperature is 260 ℃ and the screw rotating speed is 120 rpm, and carrying out extrusion, granulation and drying to obtain the highlight flame-retardant polypropylene material.
The antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
The products obtained in the three examples and the three comparative examples were subjected to a vertical burning grade test in accordance with GB/T2408-.
Table 1 results of performance testing
As can be seen from the test results of the three groups of examples and the three groups of comparative examples, the flame retardance, the glossiness, the mechanical property and the thermal oxidation aging resistance of the three groups of examples are all obviously superior to those of the three groups of comparative examples, and are far superior to those of polypropylene, which shows that 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide prepared by the reaction of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 1,3:2, 4-di-p-methyl benzylidene sorbitol, polypropylene grafted maleic anhydride, an antioxidant and polypropylene are subjected to primary mixing, melt blending, extrusion and granulation, can be prepared into polypropylene materials with excellent flame retardance, higher glossiness, better mechanical property and stronger thermo-oxidative aging resistance.
While the foregoing description shows and describes the preferred embodiments of the present invention, it is to be understood that the invention is not limited to the forms disclosed herein, but is not to be construed as excluding other embodiments and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as described herein, commensurate with the above teachings, or the skill or knowledge of the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (3)
1. A preparation method of a highlight flame-retardant polypropylene material is characterized by comprising the following steps: 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 1,3:2, 4-di-p-methyl benzylidene sorbitol, polypropylene grafted maleic anhydride, an antioxidant and polypropylene which are prepared by the reaction of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and glycidol are primarily mixed, and then the mixture is prepared by melt blending, extrusion and granulation; the method specifically comprises the following steps:
(1) adding 1-2 g of glycidol into 200-500 mL of N, N-dimethylformamide, magnetically stirring at room temperature for 20-60 min, heating to 80-120 ℃, adding 3-12 g of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, continuously magnetically stirring until the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is fully dissolved, continuously magnetically stirring for reacting for 6-12 h, pouring the reaction solution into a large amount of water, filtering the separated solid, washing and drying to prepare 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol;
(2) 10-20 parts of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide grafted glycidol, 0.05-0.4 part of 1,3:2, 4-di-p-methylbenzylidene sorbitol, 5-10 parts of polypropylene grafted maleic anhydride, 0.5-1 part of antioxidant and 100 parts of polypropylene are mixed for 10-30 min by a high-speed mixer, the initial mixture is subjected to melt blending by a double-screw extruder, the melting temperature is 200-260 ℃, the screw rotating speed is 60-120 rpm, and the highlight flame-retardant polypropylene material is prepared by extrusion, granulation and drying.
2. The preparation method of the high-gloss flame-retardant polypropylene material according to claim 1, wherein the preparation method comprises the following steps: the antioxidant is a compound system of an antioxidant 1010 and an antioxidant 168, wherein the weight ratio of the antioxidant 1010 to the antioxidant 168 is 1: 2.
3. The preparation method of the high-gloss flame-retardant polypropylene material according to claim 1, wherein the preparation method comprises the following steps: in the polypropylene grafted maleic anhydride, the weight percentage of the maleic anhydride is 0.8%.
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| EP0005441A1 (en) * | 1978-04-14 | 1979-11-28 | Ciba-Geigy Ag | Aminodibenzoxaphosphorines, process for their preparation and their use as stabilisators |
| CN104231431A (en) * | 2014-08-27 | 2014-12-24 | 上海日之升新技术发展有限公司 | High-glossiness flame-retardant scratch-resistant polypropylene composition and preparation method thereof |
| CN111205557A (en) * | 2020-02-28 | 2020-05-29 | 贵州民族大学 | Polypropylene, phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant composite material and preparation method and application thereof |
| CN111961288A (en) * | 2020-08-26 | 2020-11-20 | 东莞市鑫塑源塑胶科技有限公司 | High-gloss high-temperature-resistant heat-resistant oxidation polypropylene composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI229676B (en) * | 2003-04-09 | 2005-03-21 | Fdc Lees Chemical Industry Co | Novel phosphonite-based compounds, and their preparation method and use as stabilizer |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0005441A1 (en) * | 1978-04-14 | 1979-11-28 | Ciba-Geigy Ag | Aminodibenzoxaphosphorines, process for their preparation and their use as stabilisators |
| CN104231431A (en) * | 2014-08-27 | 2014-12-24 | 上海日之升新技术发展有限公司 | High-glossiness flame-retardant scratch-resistant polypropylene composition and preparation method thereof |
| CN111205557A (en) * | 2020-02-28 | 2020-05-29 | 贵州民族大学 | Polypropylene, phosphaphenanthrene and polyphosphazene double-base synergistic flame-retardant composite material and preparation method and application thereof |
| CN111961288A (en) * | 2020-08-26 | 2020-11-20 | 东莞市鑫塑源塑胶科技有限公司 | High-gloss high-temperature-resistant heat-resistant oxidation polypropylene composite material and preparation method thereof |
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