CN113549310B - Low-smoke flame-retardant polylactic acid composite material and preparation method thereof - Google Patents
Low-smoke flame-retardant polylactic acid composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-smoke flame-retardant polylactic acid composite material and a preparation method thereof, wherein the low-smoke flame-retardant polylactic acid composite material is prepared by banburying and hot press molding by taking 85% of polylactic acid, 13-14.8% of silica gel microencapsulated ammonium polyphosphate and 0.2-2% of hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheets as raw materials, wherein the sum of the weight percentages is 100%. The low-smoke flame-retardant polylactic acid composite material has both condensed phase flame-retardant and gas phase flame-retardant mechanisms, and can obviously reduce heat and toxic smoke released during the combustion of polylactic acid, thereby obviously improving the fire safety performance of polylactic acid.
Description
Technical Field
The invention belongs to the field of preparation of flame-retardant materials, and particularly relates to a low-smoke flame-retardant polylactic acid composite material and a preparation method thereof.
Background
The polylactic acid has the advantages of no toxicity, high transparency, high strength, good biocompatibility, easy processing and the like, and is widely applied to the fields of packaging, electronic and electrical industry, biomedicine, transportation and the like. However, polylactic acid is extremely easy to burn, releases a large amount of heat during combustion, generates a large amount of toxic and harmful smoke, seriously threatens personal safety and causes serious environmental pollution. In addition, the polylactic acid is also accompanied with serious melt dripping during combustion, and the rapid spread of fire is easily caused. These disadvantages greatly limit the application of polylactic acid materials. Therefore, it is necessary to perform a related treatment on polylactic acid to improve its fire safety.
At present, the introduction of a flame retardant is an effective measure for improving the fire safety performance of polymer materials. The fire retardant can be divided into various types such as an intumescent fire retardant, a metal oxidation fire retardant, a nanometer fire retardant and the like. The silica gel microencapsulated ammonium polyphosphate (SiAPP) is a typical intumescent flame retardant, can catalyze to form a compact carbon layer in a condensed phase stage, and can capture free radicals and dilute the concentration of combustible gas in a gas phase stage, so that the flame retardant has an excellent flame retardant effect. Gao et al introduced SiAPP into polystyrene to prepare flame retardant polystyrene composites. The results show that the incorporation of 20.0% SiAPP reduces the total heat release of polystyrene by 37.8%. Ni et al found LOI of the polyurethane composite up to 32.0% after 12.5% SiAPP incorporation. Meanwhile, the peak value of the heat release rate of the polyurethane composite material is obviously reduced by 83.2 percent compared with that of pure polyurethane. Although ammonium polyphosphate has high flame retardant efficiency, the smoke suppression and attenuation effects of silica gel microencapsulated ammonium polyphosphate are not significant. Therefore, it is necessary to combine the silica gel microencapsulated ammonium polyphosphate with other flame retardants to further improve the fire safety performance of the polymer material.
In recent years, titanium carbide nanosheets are widely used as two-dimensional nanosheet materials outside the fields of supercapacitors, electromagnetic shields, batteries and the like. In addition, the titanium carbide nanosheet has good thermal stability and low thermal conductivity, can play an excellent physical barrier function when a polymer is pyrolyzed, and effectively inhibits pyrolysis of the polymer. Meanwhile, titanium carbide can catalyze to form a compact and continuous carbon layer when the polymer is burnt, and the heat and toxic and harmful smoke released in the burning process of the polymer are obviously reduced. Therefore, the excellent flame-retardant effect of the ammonium polyphosphate of the silica gel microcapsule is combined with the efficient smoke suppression and attenuation effects of the titanium carbide nano-sheets, so that the prepared flame-retardant polymer composite material has high flame-retardant and smoke suppression and attenuation performances.
Disclosure of Invention
Aiming at the defect that a large amount of heat and toxic smoke are generated during the combustion of polylactic acid, the invention provides a low-smoke flame-retardant polylactic acid composite material and a preparation method thereof, which can effectively reduce the heat and the toxic smoke generated during the combustion of the polylactic acid and improve the fire safety performance of the polylactic acid.
In order to achieve the purpose, the invention adopts the following technical scheme:
a low-smoke flame-retardant polylactic acid composite material comprises the following raw materials in percentage by weight: 85% of polylactic acid, 13-14.8% of ammonium polyphosphate microencapsulated by silica gel, 0.2-2% of titanium carbide nano-sheet functionalized and modified by hexadecyl dimethyl benzyl ammonium chloride, and the sum of the polylactic acid, the ammonium polyphosphate and the hexadecyl dimethyl benzyl ammonium chloride is 100%.
Wherein the preparation steps of the silica gel microencapsulated ammonium polyphosphate are as follows:
a. adding 150 ml of absolute ethyl alcohol and 50 ml of deionized water into a three-mouth bottle, mechanically stirring and mixing, and heating to 45 ℃ to obtain a solution A;
b. adding 50 g of ammonium polyphosphate and 0.5 g of emulsifier OP-10 into the solution A, adding a certain amount of ammonia water to adjust the pH value of the solution to 9-10, and mechanically stirring the mixed solution for 5 minutes to obtain a solution B;
c. slowly adding 10 g of tetraethyl orthosilicate into the solution B within 30 minutes, and then mechanically stirring for 4 hours to obtain a solution C;
d. and after the solution C is cooled, filtering, washing the solid by deionized water and absolute ethyl alcohol, and drying the solid in a drying oven at the temperature of 80 ℃ for 24 hours to obtain the silica gel microencapsulated ammonium polyphosphate (SiAPP).
The preparation steps of the hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheet are as follows:
a. adding the dispersion containing the titanium carbide nanosheets into a three-neck flask, and then ultrasonically stirring for 10 minutes under the ice bath condition to obtain a dispersion A;
b. dropwise adding hexadecyl dimethyl benzyl ammonium chloride into the dispersion liquid A according to the mass ratio of the hexadecyl dimethyl benzyl ammonium chloride to the titanium carbide nanosheets being 2:1, and stirring for 2 hours under the nitrogen condition to obtain dispersion liquid B;
c. and centrifuging the dispersion liquid B, washing the solid with deionized water and absolute ethyl alcohol, and drying the solid in a vacuum drying oven at the temperature of 80 ℃ for 24 hours to obtain the hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheet.
The dispersion liquid containing the titanium carbide nanosheets is prepared through the following steps:
a. slowly adding 1.56 g of lithium fluoride and 1 g of carbon-aluminum-titanium into 20 ml of hydrochloric acid under the condition of magnetic stirring, and reacting for 48 hours at 35 ℃ to obtain a solution A;
b. and (3) washing the solution A with deionized water to be neutral, adding a certain amount of deionized water, carrying out ultrasonic stirring in an ice bath for 30 minutes, centrifuging, and taking supernatant to obtain the dispersion containing the titanium carbide nanosheets.
The preparation method of the low-smoke flame-retardant polylactic acid composite material comprises the steps of weighing polylactic acid, silica gel microencapsulated ammonium polyphosphate and hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheets in proportion, placing the titanium carbide nanosheets into an internal mixer, internally mixing the titanium carbide nanosheets for 10 minutes at 180 ℃, and then hot-pressing the titanium carbide nanosheets in a flat vulcanizing machine at 180 ℃ to obtain the low-smoke flame-retardant polylactic acid composite material.
The invention has the following advantages and beneficial effects:
the invention integrates condensed phase flame retardant and gas phase flame retardant mechanisms into a whole, so that the prepared polylactic acid composite material has excellent flame retardant, smoke suppression and attenuation performances, the fire safety performance of the polylactic acid is obviously improved, and the polylactic acid composite material has the advantages of lower preparation cost, simple preparation process and good application prospect.
Drawings
FIG. 1 is a heat and gas release curve of a low-smoke flame-retardant polylactic acid composite material in a combustion process: wherein a is the rate of heat release; b is the total heat release amount; c is the smoke release rate; d is the total smoke release.
FIG. 2 is a photograph of a sample of PLA7 obtained in comparative example 3 after hot melt pressing.
Detailed Description
The technical solution of the present invention is clearly and completely described below with reference to specific embodiments. Of course, the described embodiments are only some embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
The preparation method of the silica gel microencapsulated ammonium polyphosphate comprises the following steps:
a. adding 150 ml of absolute ethyl alcohol and 50 ml of deionized water into a three-mouth bottle, mechanically stirring and mixing, and heating to 45 ℃ to obtain a solution A;
b. adding 50 g of ammonium polyphosphate and 0.5 g of emulsifier OP-10 into the solution A, adding a certain amount of ammonia water to adjust the pH value of the solution to 9-10, and mechanically stirring the mixed solution for 5 minutes to obtain a solution B;
c. slowly adding 10 g of tetraethyl orthosilicate into the solution B within 30 minutes, and then mechanically stirring for 4 hours to obtain a solution C;
d. and after the solution C is cooled, filtering, washing the solid by deionized water and absolute ethyl alcohol, and drying the solid in a drying oven at the temperature of 80 ℃ for 24 hours to obtain the silica gel microencapsulated ammonium polyphosphate (SiAPP).
The preparation method of the hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheet comprises the following steps:
a. slowly adding 1.56 g of lithium fluoride and 1 g of carbon-aluminum-titanium into 20 ml of hydrochloric acid under the condition of magnetic stirring, and reacting for 48 hours at 35 ℃ to obtain a solution A;
b. washing the solution A with deionized water to neutrality, adding a certain amount of deionized water, carrying out ice-bath ultrasonic stirring for 30 minutes, centrifuging, and taking supernatant to obtain dispersion containing titanium carbide nanosheets;
c. adding the obtained dispersion containing the titanium carbide nanosheets into a three-neck flask, and then ultrasonically stirring for 10 minutes under the ice bath condition to obtain a dispersion B;
d. dropwise adding hexadecyl dimethyl benzyl ammonium chloride into the dispersion liquid B according to the mass ratio of the hexadecyl dimethyl benzyl ammonium chloride to the titanium carbide nanosheets being 2:1, and stirring for 2 hours under the nitrogen condition to obtain dispersion liquid C;
e. and (3) centrifuging the dispersion liquid C, washing the solid with deionized water and absolute ethyl alcohol, and drying the solid in a vacuum drying oven at the temperature of 80 ℃ for 24 hours to obtain the hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheet.
Example 1:
a low-smoke flame-retardant polylactic acid composite material is prepared according to the following specific steps:
a. weighing 0.2 part of hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheet, 14.8 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. placing the weighed titanium carbide nanosheets functionally modified by the hexadecyl dimethyl benzyl ammonium chloride, the ammonium polyphosphate microencapsulated by the silica gel and the polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the low-smoke flame-retardant polylactic acid composite material (PLA 3).
Example 2:
a low-smoke flame-retardant polylactic acid composite material is prepared according to the following specific steps:
a. weighing 0.5 part of hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheet, 14.5 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. placing the weighed titanium carbide nanosheets functionally modified by the hexadecyl dimethyl benzyl ammonium chloride, the ammonium polyphosphate microencapsulated by the silica gel and the polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the low-smoke flame-retardant polylactic acid composite material (PLA 4).
Example 3:
a low-smoke flame-retardant polylactic acid composite material is prepared according to the following specific steps:
a. weighing 1 part of hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheet, 14 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. placing the weighed titanium carbide nanosheets functionally modified by the hexadecyl dimethyl benzyl ammonium chloride, the ammonium polyphosphate microencapsulated by the silica gel and the polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the low-smoke flame-retardant polylactic acid composite material (PLA 5).
Example 4:
a low-smoke flame-retardant polylactic acid composite material is prepared according to the following specific steps:
a. weighing 2 parts of hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheets, 13 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. placing the weighed titanium carbide nanosheets functionally modified by the hexadecyl dimethyl benzyl ammonium chloride, the ammonium polyphosphate microencapsulated by the silica gel and the polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the low-smoke flame-retardant polylactic acid composite material (PLA 6).
Comparative example 1:
pure polylactic acid is prepared according to the following steps:
a. weighing 100 parts of polylactic acid;
b. placing the weighed polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the pure polylactic acid (PLA 1).
Comparative example 2:
the flame-retardant polylactic acid composite material is prepared according to the following steps:
a. weighing 15 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. and placing the weighed ammonium polyphosphate microencapsulated by the silica gel and the polylactic acid into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the flame-retardant polylactic acid composite material (PLA 2).
Comparative example 3:
the flame-retardant polylactic acid composite material is prepared according to the following steps:
a. weighing 5 parts of hexadecyl dimethyl benzyl ammonium chloride functionalized modified titanium carbide nanosheets, 10 parts of silica gel microencapsulated ammonium polyphosphate and 85 parts of polylactic acid;
b. placing the weighed titanium carbide nanosheets functionally modified by the hexadecyl dimethyl benzyl ammonium chloride, ammonium polyphosphate microencapsulated by silica gel and polylactic acid into an internal mixer, carrying out internal mixing for 10 minutes at 180 ℃, and then placing the internally mixed sample into a flat vulcanizing machine at 180 ℃ for hot press molding to obtain the flame-retardant polylactic acid composite material (PLA 7).
The fire safety performance of the materials prepared in examples 1 to 4 and comparative examples 1 to 2 was analyzed. An analysis device: a CFZ-2 type horizontal vertical combustion tester and a cone calorimeter; the heat radiation value of the cone calorimeter is 35kW/m2. The results are shown in tables 1-2 and FIG. 1.
TABLE 1 UL-94 test data for low smoke flame retardant polylactic acid composites
TABLE 2 Low Smoke flame retardant polylactic acid composite material having a heat flux of 35kW/m2Cone calorimeter test data under conditions
As can be seen from Table 1, after the ammonium polyphosphate microencapsulated by silica gel and the titanium carbide nanosheet functionally modified by hexadecyl dimethyl benzyl are introduced, the obtained polylactic acid composite material has no phenomenon of melt dripping after combustion, and the UL-94 of all the polylactic acid composite materials reach the V-0 grade. Particularly, the LOI value of the polylactic acid composite material prepared by introducing 13% of silicon gel microencapsulated ammonium polyphosphate and 2% of hexadecyl dimethyl benzyl functionalized modified titanium carbide nanosheets is as high as 33.3%.
As can be calculated from table 2 and fig. 1, compared with pure polylactic acid, the peak value of the heat release rate and the total heat release amount of the polylactic acid composite material prepared by introducing 13.0% of silica gel microencapsulated ammonium polyphosphate and 2.0% of hexadecyldimethylbenzyl ammonium chloride functionalized modified titanium carbide nanosheets are respectively reduced by 49.8% and 31.9%; the peak smoke release rate and the total smoke release were reduced by 60.8% and 52.7%, respectively.
As can be seen from fig. 2, when the addition amount of the titanium carbide nanosheet functionally modified by the hexadecyl dimethyl benzyl ammonium chloride is increased to 2.0% and the addition amount of the ammonium polyphosphate microencapsulated by the silica gel is reduced to 10.0%, due to the antagonistic action of mutual catalysis between the modified titanium carbide nanosheet and the ammonium polyphosphate microencapsulated by the silica gel, the molten drop of the composite material sample in the banburying and hot melt-pressing processes is abnormal and the complete polylactic acid composite material cannot be prepared.
From the analysis of the data, the heat and toxic smoke released by the prepared polylactic acid composite material during combustion are effectively reduced due to the blocking and catalytic effects of the modified titanium carbide, the char formation and free radical interruption effects of the phosphorus-containing flame retardant and the synergistic effect of the modified titanium carbide and the phosphorus-containing flame retardant, and the fire safety performance of the polylactic acid is improved.
The low-smoke flame-retardant polylactic acid composite material and the preparation method thereof provided by the invention are described in detail above. The preparation and use of the present invention are illustrated herein using specific examples, which are merely provided to aid in the understanding of the method and core concepts of the present invention. It should be noted that, for those skilled in the art, it is possible to make various modifications and improvements to the present invention without departing from the principle of the present invention, and those modifications and improvements should fall within the protection scope of the claims of the present invention.
Claims (2)
1. A low-smoke flame-retardant polylactic acid composite material is characterized in that: the raw materials are as follows by weight percent: 85% of polylactic acid, 13-14.8% of ammonium polyphosphate microencapsulated by silica gel and 0.2-2% of titanium carbide nano-sheets functionally modified by hexadecyl dimethyl benzyl ammonium chloride, wherein the sum of the polylactic acid, the ammonium polyphosphate and the hexadecyl dimethyl benzyl ammonium chloride is 100%;
the preparation method of the silica gel microencapsulated ammonium polyphosphate comprises the following steps:
a. stirring and mixing 150 ml of absolute ethyl alcohol and 50 ml of deionized water, and heating to 45 ℃ to obtain a solution A;
b. adding 50 g of ammonium polyphosphate and 0.5 g of emulsifier OP-10 into the solution A, adding a certain amount of ammonia water to adjust the pH value of the solution to 9-10, and mechanically stirring the mixed solution for 5 minutes to obtain a solution B;
c. slowly adding 10 g of tetraethyl orthosilicate into the solution B within 30 minutes, and mechanically stirring for 4 hours to obtain a solution C;
d. after the solution C is cooled, filtering, washing the solid by deionized water and absolute ethyl alcohol, and drying the solid for 24 hours at 80 ℃ to obtain the silica gel microencapsulated ammonium polyphosphate;
the preparation steps of the hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheet are as follows:
a. ultrasonically stirring the dispersion liquid containing the titanium carbide nanosheets for 10 minutes under the ice bath condition to obtain a dispersion liquid A;
b. dropwise adding hexadecyl dimethyl benzyl ammonium chloride into the dispersion liquid A according to the mass ratio of the hexadecyl dimethyl benzyl ammonium chloride to the titanium carbide nanosheets being 2:1, and stirring for 2 hours under the nitrogen condition to obtain dispersion liquid B;
c. centrifuging the dispersion liquid B, washing the solid with deionized water and absolute ethyl alcohol, and drying the solid at 80 ℃ for 24 hours to obtain the hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheet;
the dispersion liquid containing the titanium carbide nanosheets is prepared through the following steps:
a. slowly adding 1.56 g of lithium fluoride and 1 g of carbon-aluminum-titanium into 20 ml of hydrochloric acid under the condition of magnetic stirring, and reacting for 48 hours at 35 ℃ to obtain a solution A;
b. and (3) washing the solution A with deionized water to be neutral, adding a certain amount of deionized water, carrying out ultrasonic stirring in an ice bath for 30 minutes, centrifuging, and taking supernatant to obtain the dispersion containing the titanium carbide nanosheets.
2. A method for preparing a low smoke flame retardant polylactic acid composite material according to claim 1, which is characterized in that: weighing polylactic acid, silica gel microencapsulated ammonium polyphosphate and hexadecyl dimethyl benzyl ammonium chloride functionalized and modified titanium carbide nanosheets according to the proportion, placing the titanium carbide nanosheets into an internal mixer, internally mixing for 10 minutes at 180 ℃, and then hot-pressing and molding in a flat vulcanizing machine at 180 ℃ to obtain the low-smoke flame-retardant polylactic acid composite material.
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