CN111621137A - Low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and preparation method thereof - Google Patents
Low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and a preparation method thereof, wherein the composite material comprises the following components in parts by weight: 58.8-60 parts of thermoplastic polyurethane, 0-0.92 part of titanium carbide nanosheet, 0-1.2 parts of graphite oxide, 250 parts of N-N-dimethylformamide and 0-4 parts of hydrazine hydrate. The flame-retardant thermoplastic polyurethane composite material provided by the invention integrates the physical barrier effect of the titanium carbide nanosheets and the graphene and the condensed phase flame-retardant effect, and has excellent flame-retardant performance and smoke suppression and toxicity reduction performance.
Description
Technical Field
The invention belongs to the field of preparation of flame retardants and flame retardant materials, and particularly relates to a low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material and a preparation method thereof.
Technical Field
Thermoplastic Polyurethane (TPU) is a polymeric material that has both the processability of thermoplastic polymers and the mechanical properties of vulcanized rubber. Due to excellent wear resistance, corrosion resistance and self-lubricating property, the thermoplastic polyurethane has wide application in many fields such as automobile parts, industries of electricity, electronics and the like, mechanical transmission parts, household, cosmetics and the like. However, thermoplastic polyurethane materials are extremely easy to burn, emit a large amount of heat during burning, generate a large amount of smoke, generate toxic and harmful gases such as CO and HCN, are harmful to human health, and pollute the environment to a certain extent. In addition, thermoplastic polyurethane can generate serious melt dripping phenomenon during combustion, so that fire spreading is easy to occur during combustion. These disadvantages have largely limited the widespread use of thermoplastic polyurethane materials. Therefore, the development of low-smoke, low-toxicity flame-retardant thermoplastic polyurethane materials is imperative.
At present, aiming at the problem of low fire safety performance of thermoplastic polyurethane materials, corresponding flame retardants have been developed in the world, and can be mainly divided into two categories, namely additive flame retardants and reactive flame retardants. The additive flame-retardant method is that the flame retardant is added into the thermoplastic polyurethane material in a physically dispersed form, and the flame retardant does not react with the thermoplastic polyurethane matrix. The method has the advantages of low cost, easy processing and production and the like, and most of the flame-retardant materials are prepared by the method at present. The two-dimensional lamellar flame retardant is one of additive flame retardants, common two-dimensional lamellar materials comprise montmorillonite, metal double-layer hydroxide, boron nitride, molybdenum disulfide and the like, and the montmorillonite, the metal double-layer hydroxide, the boron nitride, the molybdenum disulfide and the like can be independently added into a thermoplastic polyurethane material as a flame retardant and can also be compounded with other flame retardants to further prepare flame retardants with excellent synergistic performance. However, when the two-dimensional sheet material is added into thermoplastic polyurethane, a large amount of toxic smoke is generated, and the flame retardant efficiency is low. Therefore, the development of new low-smoke low-toxicity flame-retardant thermoplastic polyurethane materials is not slow.
The titanium carbide nanosheet is used as a two-dimensional lamellar material, and has very wide application prospect in the fields of super capacitors, lithium (or sodium) ion batteries, electromagnetic shielding and the like due to inherent high metal conductivity, excellent mechanical stability and intercalation capability. In addition, titanium carbide has good thermal stability and low lamellar thermal conductivity, and can play a lamellar barrier effect in the pyrolysis and combustion processes of polymer materials. Meanwhile, the transition metal element titanium can promote the polymer matrix to form a compact carbon layer, can effectively prevent the exchange of substances and energy between the combustion zone and the polymer matrix, inhibit the degradation of the polymer and simultaneously prevent the release of toxic smoke.
Graphene is sp in two-dimensional plane2The hybridized carbon atoms are orderly arranged to form the nanometer material. As a typical two-dimensional material, the composite material has excellent catalytic carbon formation effect and high-efficiency lamellar physical barrier effect, is often used as a flame retardant additive of a polymer and also has certain flame retardant effect.
Disclosure of Invention
The invention aims to provide a low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material, which has high-efficiency flame-retardant performance and smoke suppression and toxicity reduction performance by introducing proper titanium carbide nanosheet/graphene hybrid.
The second purpose of the invention is to provide a preparation method of the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
one aspect of the invention provides a low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material, which comprises the following components in parts by weight: 58.8-60 parts of thermoplastic polyurethane, 0-0.92 part of titanium carbide nanosheet, 0-1.2 parts of graphite oxide, 250 parts of N-N-dimethylformamide and 0-4 parts of hydrazine hydrate;
the titanium carbide nanosheet is prepared through the following steps:
slowly adding 1.56 g of lithium fluoride and 1 g of carbon-aluminum-titanium into a centrifugal tube filled with 20 ml of hydrochloric acid under magnetic stirring, reacting for 48 hours at 35 ℃ to obtain a titanium carbide solution, adding a certain amount of deionized water after the titanium carbide solution is washed to be neutral, ultrasonically stirring for 30 minutes under an ice bath condition, centrifuging, and taking supernatant to obtain the titanium carbide nanosheet.
The graphite oxide is prepared by the following steps:
a. under the conditions of magnetic stirring and ice bath, slowly adding 230 ml of concentrated sulfuric acid, 10 g of graphite powder, 5 g of sodium nitrate and 30 g of potassium permanganate into a 2L beaker filled with a certain amount of deionized water in sequence, then placing the beaker into an oil bath pot, and stirring for 30 minutes at 35 ℃ to obtain a mixed solution;
b. slowly adding 460 ml of deionized water into the mixed solution, heating an oil bath to 95 ℃, stirring for 15 minutes, adding 700 ml of warm water into a beaker, reacting for a certain time, adding 25 ml of hydrogen peroxide into the beaker, carrying out centrifugal washing after the reaction is finished, and obtaining Graphite Oxide (GO) after the pH of the solution is close to neutral.
Another aspect of the present invention provides a method for preparing the flame retardant thermoplastic polyurethane composite material with low smoke and low toxicity, comprising the following steps:
(1) weighing thermoplastic polyurethane, titanium carbide nanosheets, graphite oxide, N-N-dimethylformamide and hydrazine hydrate as raw material groups;
(2) putting titanium carbide nanosheets and graphite oxide into a 100 ml three-neck flask, and ultrasonically stirring for 0.5 hour to obtain a solution A;
(3) dropwise adding hydrazine hydrate into the solution A, and ultrasonically stirring for 10 minutes to obtain a solution B;
(4) transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
(5) carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the solution C in a vacuum drying oven at 70 ℃ for drying for 24 hours to obtain a substance D;
(6) adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
(7) adding N-N-dimethylformamide into a 500-milliliter three-neck flask, placing the flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
(8) adding the solution E into the solution F, and ultrasonically stirring for 1 hour to obtain a solution G;
(9) adding the solution G into 1000 ml of deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the solution G in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
(10) and (3) banburying the substance H at 190 ℃ and pressing a plate to obtain the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material.
Due to the adoption of the technical scheme, the invention has the following advantages and beneficial effects:
the design integrates the physical barrier effect and the condensed phase flame retardant effect, the manufacturing process is simple, the cost is lower, the obtained thermoplastic polyurethane composite material has high-efficiency flame retardant performance and smoke suppression and attenuation performance, and the fire safety performance of the thermoplastic polyurethane material is greatly improved.
Drawings
FIG. 1 is a graph of heat release versus smoke release of a low smoke, low toxicity, flame retardant thermoplastic polyurethane composite during combustion;
FIG. 2 is a graph of the gas release profile of a low smoke, low toxicity, flame retardant thermoplastic polyurethane composite during combustion.
Detailed description of the preferred embodiments
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.
Example 1:
a low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material is synthesized according to the following steps:
a. weighing 58.8 parts of thermoplastic polyurethane, 0.92 part of titanium carbide nanosheet, 0.28 part of graphite oxide, 250 parts of N-N-dimethylformamide and 3 parts of hydrazine hydrate as raw material groups;
b. putting titanium carbide nanosheets and graphite oxide into a 100 ml three-neck flask, and ultrasonically stirring for 0.5 hour to obtain a solution A;
c. dropwise adding hydrazine hydrate into the solution A, and ultrasonically stirring for 10 minutes to obtain a solution B;
d. transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
e. carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the solution C in a vacuum drying oven at 70 ℃ for drying for 24 hours to obtain a substance D;
f. adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
g. adding N-N-dimethylformamide into a 500-milliliter three-neck flask, placing the flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
h. adding the solution E into the solution F, and ultrasonically stirring for 1 hour to obtain a solution G;
i. adding the solution G into 1000 ml of deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the solution G in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
j. banburying and pressing the substance H at 190 ℃ to obtain the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material (TPU/Ti)3C2Tx-rGO-2.0）。
Example 2:
a low-smoke low-toxicity flame-retardant thermoplastic polyurethane material is synthesized according to the following steps:
a. weighing 59.4 parts of thermoplastic polyurethane, 0.46 part of titanium carbide nanosheet, 0.14 part of graphite oxide, 250 parts of N-N-dimethylformamide and 2 parts of hydrazine hydrate as raw material groups;
b. putting titanium carbide nanosheets and graphite oxide into a 100 ml three-neck flask, and ultrasonically stirring for 0.5 hour to obtain a solution A;
c. dropwise adding hydrazine hydrate into the solution A, and ultrasonically stirring for 10 minutes to obtain a solution B;
d. transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
e. carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the solution C in a vacuum drying oven at 70 ℃ for drying for 24 hours to obtain a substance D;
f. adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
g. adding N-N-dimethylformamide into a 500-milliliter three-neck flask, placing the flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
h. adding the solution E into the solution F, and ultrasonically stirring for 1 hour to obtain a solution G;
i. adding the solution G into 1000 ml of deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the solution G in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
j. banburying and pressing the substance H at 190 ℃ to obtain the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material (TPU/Ti)3C2Tx-rGO-1.0）。
Example 3:
a low-smoke low-toxicity flame-retardant thermoplastic polyurethane material is synthesized according to the following steps:
a. weighing 59.7 parts of thermoplastic polyurethane, 0.23 part of titanium carbide nanosheet, 0.07 part of graphite oxide, 250 parts of N-N-dimethylformamide and 1 part of hydrazine hydrate as raw material groups;
b. putting titanium carbide nanosheets and graphite oxide into a 100 ml three-neck flask, and ultrasonically stirring for 0.5 hour to obtain a solution A;
c. dropwise adding hydrazine hydrate into the solution A, and ultrasonically stirring for 10 minutes to obtain a solution B;
d. transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
e. carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the solution C in a vacuum drying oven at 70 ℃ for drying for 24 hours to obtain a substance D;
f. adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
g. adding N-N-dimethylformamide into a 500-milliliter three-neck flask, placing the flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
h. adding the solution E into the solution F, and ultrasonically stirring for 1 hour to obtain a solution G;
i. adding the solution G into 1000 ml of deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the solution G in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
j. banburying and pressing the substance H at 190 ℃ to obtain the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material (TPU/Ti)3C2Tx-rGO-0.5）。
Comparative example 1:
a thermoplastic polyurethane material is synthesized according to the following steps:
a. weighing 60 parts of thermoplastic polyurethane as a raw material group;
b. and (3) banburying and pressing the thermoplastic polyurethane at 190 ℃ to obtain the plastic polyurethane material (TPU).
Comparative example 2:
a flame-retardant thermoplastic polyurethane material is synthesized according to the following steps:
a. weighing 58.8 parts of thermoplastic polyurethane, 1.2 parts of graphite oxide, 250 parts of N-N-dimethylformamide and 4 parts of hydrazine hydrate as raw material groups;
b. placing graphite oxide in a 100 ml three-neck flask, and ultrasonically stirring for 0.5 hour to obtain a solution A;
c. dropwise adding hydrazine hydrate into the solution A obtained in the step B, and ultrasonically stirring for 10 minutes to obtain a solution B;
d. transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
e. carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then placing the solution C in a vacuum drying oven at 70 ℃ for drying for 24 hours to obtain a substance D;
f. adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
g. adding N-N-dimethylformamide into a 500-milliliter three-neck flask, placing the flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
h. adding the solution G into the thermoplastic polyurethane solution obtained in the step, and ultrasonically stirring for 1 hour to obtain a solution G;
i. adding the solution H into 1000 ml of deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the thermoplastic polyurethane composite material in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
j. and (3) banburying and pressing the substance H at 190 ℃ to obtain the flame-retardant thermoplastic polyurethane composite material (TPU/rGO-2.0).
Cone calorimeter analysis was performed on the low smoke, low toxicity flame retardant thermoplastic polyurethane composites prepared in examples 1-3 and comparative examples 1-2. An analysis device: a cone calorimeter; heat radiation value: 35kW/m2。
FIG. 1 is a heat release and smoke release curve of a low smoke, low toxicity, flame retardant thermoplastic polyurethane composite during combustion: (a) the rate of heat release; (b) total heat release; (c) smoke generation rate (d) total smoke generation, fig. 2 is a gas release curve of the low smoke, low toxicity flame retardant thermoplastic polyurethane composite material during combustion: (a) the rate of carbon monoxide release; (b) total carbon monoxide release; (c) rate of carbon dioxide release (d) total carbon dioxide release; as can be calculated from table 2 and fig. 1-2, the total heat release of the sample was reduced by 28%, 17% and 25% respectively after adding 2.0%, 1.0% and 0.5% of titanium carbide nanosheet/graphene hybrid relative to the TPU sample; the total smoke generation is respectively reduced by 59 percent, 9 percent and 20 percent; the total carbon monoxide production is respectively reduced by 46 percent, 8 percent and 40 percent; the total carbon dioxide production was reduced by 30%, 17% and 26%, respectively.
When the added titanium carbide nanosheet/graphene hybrid is 2.0%, the thermoplastic polyurethane composite material has the best flame-retardant, smoke-suppressing and toxicity-reducing effects; the physical barrier effect of the titanium carbide nanosheet/graphene hybrid and the catalytic carbonization effect of the titanium carbide nanosheet are the main reasons for remarkably improving the flame retardant, smoke suppression and toxicity reduction performances of the thermoplastic polyurethane.
From the analysis of the data, the flame retardant property and the smoke suppression and attenuation property of the thermoplastic polyurethane can be effectively improved by adding a certain amount of titanium carbide nanosheet/graphene hybrid.
The flame-retardant thermoplastic polyurethane composite material with low smoke and low toxicity and the preparation method thereof provided by the invention are introduced 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 (4)
1. A low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material is characterized in that: the paint comprises the following components in parts by weight: 58.8-60 parts of thermoplastic polyurethane, 0-0.92 part of titanium carbide nanosheet, 0-1.2 parts of graphite oxide, 250 parts of N-N-dimethylformamide and 0-4 parts of hydrazine hydrate.
2. The low smoke, low toxicity, flame retardant thermoplastic polyurethane composite of claim 1, wherein: the titanium carbide nanosheet is prepared through the following steps: slowly adding lithium fluoride and carbon aluminum titanium into a hydrochloric acid solution, reacting for 48 hours at 35 ℃ to obtain a titanium carbide solution, washing the titanium carbide solution to be neutral, adding deionized water, ultrasonically stirring for 30 minutes under an ice bath condition, centrifuging, and taking supernatant to obtain the titanium carbide nanosheet.
3. The low smoke, low toxicity, flame retardant thermoplastic polyurethane composite of claim 1, wherein: the graphite oxide is prepared by the following steps:
a. under the conditions of magnetic stirring and ice bath, slowly adding concentrated sulfuric acid, graphite powder, sodium nitrate and potassium permanganate into deionized water in sequence, then placing the deionized water in an oil bath pot, and stirring the mixture for 30 minutes at the temperature of 35 ℃ to obtain a mixed solution;
b. and adding deionized water into the mixed solution, heating an oil bath to 95 ℃, stirring for 15 minutes, adding a proper amount of warm water, reacting for a certain time, finally adding hydrogen peroxide, performing centrifugal washing after the reaction is finished, and obtaining the graphite oxide after the pH of the solution is close to neutral.
4. A method for preparing a low smoke, low toxicity, flame retardant thermoplastic polyurethane composite material as claimed in any one of claims 1 to 3, wherein: comprises the following steps of (a) carrying out,
(1) weighing thermoplastic polyurethane, titanium carbide nanosheets, graphite oxide, N-N-dimethylformamide and hydrazine hydrate as raw material groups;
(2) ultrasonically stirring the titanium carbide nanosheets and the graphite oxide for 0.5 hour to obtain a solution A;
(3) dropwise adding hydrazine hydrate into the solution A, and ultrasonically stirring for 10 minutes to obtain a solution B;
(4) transferring the solution B into a reaction kettle, and reacting for 24 hours at 180 ℃ to obtain a solution C;
(5) carrying out suction filtration on the solution C, washing the solution C for a plurality of times by using deionized water and absolute ethyl alcohol, and then carrying out vacuum drying for 24 hours at 70 ℃ to obtain a substance D;
(6) adding the substance D into 25 ml of absolute ethyl alcohol, and ultrasonically stirring for 3 minutes to obtain a solution E;
(7) adding N-N-dimethylformamide into a three-neck flask, placing the three-neck flask in an oil bath pot, slowly adding thermoplastic polyurethane after the temperature of the oil bath pot is raised to 80 ℃, and mechanically stirring for 2 hours to obtain a solution F;
(8) adding the solution E into the solution F, and ultrasonically stirring for 1 hour at room temperature to obtain a solution G;
(9) adding the solution G into deionized water, and after the thermoplastic polyurethane composite material is separated out, placing the solution G in a drying oven at 80 ℃ for drying for 48 hours to obtain a substance H;
(10) and (3) banburying the substance H at 190 ℃ and pressing a plate to obtain the low-smoke low-toxicity flame-retardant thermoplastic polyurethane composite material.
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| CHUAN LIU: "Creating MXene/reduced graphene oxide hybrid towards highly fire safe", 《COMPOSITES PART B ENGINEERING》 * |
| LINGXIN H: "Large-scale production of simultaneously exfoliated and Functionalized Mxenes as promising flame retardant for polyurethane", 《COMPOSITES PART B ENGINEERING》 * |
| XIAOLONG WANG: "The effect of two-dimensional d-Ti3C2 on the mechanical and", 《POLYMER COMPOSITES》 * |
| 胡静: "Self-assembled fabrication and flame-retardant propertiesof reduced graphene oxide/waterborne polyurethane nanocomposites", 《JOURNAL OF THERMAL ANALYSIS AND CALORIMETR》 * |
| 胡静: "加压密闭氧化石墨烯/水性聚氨酯纳米复合材料的制备及阻燃性能", 《高分子材料科学与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112724462A (en) * | 2020-12-29 | 2021-04-30 | 合肥学院 | Titanium carbide nano powder for ABS flame retardation, smoke suppression and toxicity reduction and preparation method thereof |
| CN112724462B (en) * | 2020-12-29 | 2022-05-10 | 合肥学院 | Titanium carbide nano powder for ABS flame retardation, smoke suppression and toxicity reduction and preparation method thereof |
| CN112941896A (en) * | 2021-03-05 | 2021-06-11 | 华南理工大学 | Multifunctional flame-retardant cotton fabric and preparation method and application thereof |
| CN113549310A (en) * | 2021-08-12 | 2021-10-26 | 福州大学 | Low-smoke flame-retardant polylactic acid composite material and preparation method thereof |
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