Flame retardant material and method for its production

Abstract

The application relates to the technical field of flame-retardant materials, and discloses a flame-retardant material and a preparation method thereof. The flame-retardant material comprises the following components by weight: nylon 40-85 parts, diisobutyl aluminum hypophosphite 5-20 parts, brominated polystyrene 5-20 parts, antimony trioxide 1-3 parts, fibers 0-35 parts, and antioxidant 0.2-0.5 parts; and the antimony trioxide is composed of cubic antimony trioxide and rhombic antimony trioxide. The technical scheme solves the problem of poor flame-retardant performance of the flame-retardant material in the related art.

Description

Technical Field

[0001] This invention relates to the field of flame retardant materials technology, specifically to a flame retardant material and its preparation method. Background Technology

[0002] Nylon, as a synthetic polymer material, is widely used in many industries, such as textiles, automobiles, and electronics, thanks to its excellent mechanical properties, good wear resistance, and outstanding processing performance.

[0003] However, nylon materials have a significant drawback: poor flame retardancy. In applications with high fire protection requirements, such as construction and aerospace, this limitation restricts the further promotion and application of nylon. Adding flame retardants to nylon is a common method to improve its flame retardancy.

[0004] However, existing flame retardants present numerous problems when added to nylon. On one hand, their flame-retardant effect is limited, failing to meet increasingly stringent fire protection standards and practical application requirements. On the other hand, existing flame retardants generally suffer from agglomeration. This agglomeration makes it difficult for the flame retardant to achieve uniform dispersion within the nylon matrix, resulting in uneven distribution of flame-retardant properties within the nylon material. Furthermore, poor compatibility between the flame retardant and nylon further exacerbates agglomeration, preventing the flame retardant from fully exerting its flame-retardant effect. These problems not only affect the flame-retardant properties of nylon materials but also adversely impact their mechanical properties.

[0005] Therefore, it is essential to develop a flame-retardant material with high flame-retardant properties. Summary of the Invention

[0006] This invention proposes a flame-retardant material and its preparation method, which solves the problem of poor flame-retardant performance of flame-retardant materials in related technologies.

[0007] The technical solution of the present invention is as follows: The present invention proposes a flame retardant material comprising the following raw materials in parts by weight: 40-85 parts of nylon, 5-20 parts of aluminum diisobutylphosphite, 5-20 parts of brominated polystyrene, 1-3 parts of antimony trioxide, 0-35 parts of fiber, and 0.2-0.5 parts of antioxidant; wherein the antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide.

[0008] As a further technical solution, the mass ratio of the cubic antimony trioxide to the orthorhombic antimony trioxide is 1:2~3.

[0009] In the flame-retardant material of this invention, by adjusting the ratio of cubic antimony trioxide to orthorhombic antimony trioxide, the unique performance advantages of the two antimony trioxide crystal forms are fully utilized, enabling them to produce a synergistic effect during the flame-retardant process. This effectively improves the flame-retardant efficiency of the material, reduces the combustion rate, and decreases the release of smoke and toxic gases. Furthermore, it achieves good compatibility between antimony trioxide and other components in the system, such as aluminum diisobutylphosphite and brominated polystyrene, enhancing the stability and compatibility of the entire flame-retardant system and further improving the mechanical properties of the flame-retardant material.

[0010] The flame retardant material of the present invention incorporates an antioxidant, which can effectively capture free radicals generated during the processing and use of the material, thereby significantly delaying the oxidative degradation process of the flame retardant material. Furthermore, the antioxidant has good thermal stability and processing adaptability, can remain stable in high-temperature environments, will not decompose or fail, and will not negatively affect the processing flowability of the material. It can improve the thermal stability of the material during processing, reduce the deterioration of material properties caused by high-temperature oxidation, make the material easier to process and shape, and improve production efficiency and product quality.

[0011] The flame-retardant material of the present invention incorporates fibers, which improves the internal structure of the flame-retardant material, making it more compact. The compact internal structure makes the flame-retardant material more difficult to ignite when it encounters a flame, increasing the resistance to flame propagation. The flame needs to overcome more obstacles to spread in the material, thereby improving the overall flame-retardant performance of the material and providing a more reliable safety guarantee for the use of the material.

[0012] As a further technical solution, the nylon includes one or both of nylon 6 and nylon 66.

[0013] As a further technical solution, the antioxidant includes one or more of antioxidant 1010, antioxidant 168, and antioxidant 1076.

[0014] As a further technical solution, when the fiber is not zero, the fiber includes one or more of glass fiber, carbon fiber, and aramid fiber.

[0015] As a further technical solution, the antimony trioxide is an aminochlorobenzenesulfonamide compound composite antimony trioxide.

[0016] In the flame retardant material of the present invention, an aminochlorobenzenesulfonamide compound is used to combine with antimony trioxide to enhance the dispersibility of antimony trioxide in the matrix material, enhance the compatibility and bonding strength between antimony trioxide and the matrix material, reduce the cracking and detachment of the char layer during combustion, maintain the overall structural integrity of the material, and further improve the mechanical properties of the flame retardant material.

[0017] As a further technical solution, the aminochlorobenzenesulfonamide compound in the antimony trioxide compound includes one or two of 2-amino-4-chloro-5-methylbenzenesulfonamide and 4-amino-3-chlorobenzenesulfonamide.

[0018] As a further technical solution, the raw materials for the aminochlorobenzenesulfonamide compound composite antimony trioxide include an aminochlorobenzenesulfonamide compound and antimony trioxide in a mass ratio of 2~3:30.

[0019] In the flame retardant material of the present invention, the mass ratio of aminochlorobenzenesulfonamide compound to antimony trioxide is 2~3:30. The appropriate mass ratio allows the aminochlorobenzenesulfonamide compound to act uniformly on the surface of antimony trioxide particles, effectively preventing the agglomeration of antimony trioxide particles, thereby making them more evenly distributed in the matrix material, improving the overall performance stability of the flame retardant material, and promoting the more effective flame retardant effect of the composite antimony trioxide. This not only avoids the problems of insufficient dispersibility and poor bonding strength caused by a small amount of aminochlorobenzenesulfonamide compound, but also avoids the problems of increased cost and performance imbalance caused by an excessive amount of aminochlorobenzenesulfonamide compound.

[0020] As a further technical solution, the preparation method of the aminochlorobenzenesulfonamide compound composite antimony trioxide includes the following steps: dispersing the aminochlorobenzenesulfonamide compound in a solution, adding antimony trioxide, stirring and drying to obtain the aminochlorobenzenesulfonamide compound composite antimony trioxide.

[0021] In the flame retardant material of the present invention, an aminochlorobenzenesulfonamide compound is added to form antimony trioxide. The preparation process is simple. The aminochlorobenzenesulfonamide compound is first uniformly dispersed in a solution, and then antimony trioxide is added. The thorough stirring process helps the antimony trioxide and the aminochlorobenzenesulfonamide compound to fully contact and mix, thereby achieving the composite of aminochlorobenzenesulfonamide compound and antimony trioxide.

[0022] As a further technical solution, the stirring time is 3 to 5 hours, for example, 3 hours, 3.2 hours, 3.5 hours, 3.8 hours, 4 hours, 4.2 hours, 4.5 hours, 4.8 hours, or 5 hours, preferably 4 hours.

[0023] In the flame retardant material of the present invention, the stirring time of the aminochlorobenzenesulfonamide compound composite antimony trioxide during the preparation process is preferably 4 hours. During this stirring time, a strong force can be formed between the aminochlorobenzenesulfonamide compound molecules and the surface of the antimony trioxide particles. While ensuring product quality, this avoids energy waste and extended production cycle caused by excessive stirring time.

[0024] As a further technical solution, the mass ratio of the solution to the antimony trioxide is 3 to 10:1, for example, it can be 3:1, 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, preferably 5:1, and the solution is anhydrous ethanol.

[0025] In the flame retardant material of the present invention, the mass ratio of the solution to antimony trioxide in the preparation process of the aminochlorobenzenesulfonamide compound composite is preferably 5:1. The solution can provide sufficient space and fluidity to fully disperse the antimony trioxide particles and achieve the combination with the aminochlorobenzenesulfonamide compound. Furthermore, the 5:1 mass ratio facilitates uniform stirring and avoids increased energy consumption in subsequent drying due to excessive solution.

[0026] The present invention also proposes a method for preparing flame retardant material, comprising the following steps: weighing the raw materials, mixing them evenly, and then extruding and granulating them to obtain the flame retardant material.

[0027] The working principle and beneficial effects of this invention are as follows:

[0028] In this invention, cubic and orthorhombic antimony trioxide are used in combination to leverage their synergistic effect and improve the flame-retardant performance of the flame-retardant material. In existing technologies, antimony trioxide, as a conventional flame retardant, primarily focuses on the effect of its combination with other types of flame retardants. This invention, however, focuses on the flame-retardant influence of different crystal structures of antimony trioxide. By simultaneously adding cubic and orthorhombic antimony trioxide, this invention leverages their synergistic effect to enhance the flame-retardant efficiency throughout the combustion process, effectively suppressing flame spread, promoting the formation of a denser char layer, and ultimately improving the flame-retardant performance of the material. Detailed Implementation

[0029] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0030] In the following examples and comparative examples:

[0031] Cubic antimony trioxide: average particle size 0.75 μm;

[0032] Orthorhombic antimony trioxide: average particle size 0.8 μm;

[0033] Nylon 6: Model number YH400;

[0034] Nylon 66: Model number EPR27;

[0035] Brominated polystyrene: Model number XZ-6700.

[0036] Example 1

[0037] A method for preparing a flame-retardant material includes the following steps: weighing 40 parts of nylon 6, 5 parts of aluminum diisobutylphosphite, 5 parts of brominated polystyrene, 1 part of antimony trioxide, and 0.2 parts of antioxidant 1010, mixing them evenly, and then extruding and granulating them through a twin-screw extruder to obtain the flame-retardant material, wherein the antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide in a mass ratio of 1:2.

[0038] Example 2

[0039] A method for preparing a flame-retardant material includes the following steps: weighing 60 parts of nylon 66, 10 parts of aluminum diisobutylphosphite, 10 parts of brominated polystyrene, 2 parts of antimony trioxide, 20 parts of glass fiber, and 0.3 parts of antioxidant 168, mixing them evenly, and then extruding and granulating them through a twin-screw extruder to obtain the flame-retardant material, wherein the antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide in a mass ratio of 1:2.

[0040] Example 3

[0041] A method for preparing a flame-retardant material includes the following steps: weighing 85 parts of nylon 66, 20 parts of aluminum diisobutylphosphite, 20 parts of brominated polystyrene, 3 parts of antimony trioxide, 35 parts of carbon fiber, and 0.5 parts of antioxidant 1076, mixing them evenly, and then extruding and granulating them through a twin-screw extruder to obtain the flame-retardant material, wherein the antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide in a mass ratio of 1:2.

[0042] Example 4

[0043] Compared with Example 2, Example 4 differs in that antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide in a mass ratio of 1:3.

[0044] Example 5

[0045] A method for preparing aminochlorobenzenesulfonamide compound composite antimony trioxide includes the following steps: dispersing 0.2 parts of 2-amino-4-chloro-5-methylbenzenesulfonamide in 15 parts of anhydrous ethanol, adding 3 parts of antimony trioxide, stirring for 4 hours, and drying to obtain aminochlorobenzenesulfonamide compound composite antimony trioxide, wherein the antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide in a mass ratio of 1:3;

[0046] Compared with Example 4, Example 5 differs in that antimony trioxide is replaced with aminochlorobenzenesulfonamide compound antimony trioxide obtained by the above preparation method.

[0047] Example 6

[0048] The difference between Example 6 and Example 5 is that the amount of 2-amino-4-chloro-5-methylbenzenesulfonamide added is 0.3 parts.

[0049] Example 7

[0050] The difference between Example 7 and Example 6 is that 2-amino-4-chloro-5-methylbenzenesulfonamide is replaced with an equal amount of 4-amino-3-chlorobenzenesulfonamide.

[0051] Example 8

[0052] The difference between Example 8 and Example 6 is that 2-amino-4-chloro-5-methylbenzenesulfonamide is replaced with an equal amount of benzenesulfonamide.

[0053] Comparative Example 1

[0054] Compared with Example 2, the difference in Comparative Example 1 is that antimony trioxide is only cubic antimony trioxide.

[0055] Comparative Example 2

[0056] Compared with Example 2, the difference in Comparative Example 2 is that antimony trioxide is only orthorhombic antimony trioxide.

[0057] Experimental Example 1

[0058] The flame retardant materials prepared in Examples 1-4 and Comparative Examples 1-2 were tested for flame retardancy according to the test method specified in UL94. The sample thickness was 1.6 mm.

[0059] The test results are shown in Table 1:

[0060] Table 1. Performance test results of the flame-retardant materials prepared in Examples 1-4 and Comparative Examples 1-2

[0061]

[0062] As shown in Table 1, when the flame retardant is composed of aluminum diisobutylphosphite, brominated polystyrene, and antimony trioxide, and when the antimony trioxide is composed of cubic and orthorhombic antimony trioxide, the flame retardant performance of the flame retardant material can be improved.

[0063] Experiment Example 2

[0064] The flame-retardant materials prepared in Examples 4-8 were tested for bending strength according to the test methods specified in GB / T 9341-2008 "Determination of Flexural Properties of Plastics". The sample size was 80mm×10mm×4mm, with 5 samples in each group, and the average value of the test results was taken.

[0065] The test results are shown in Table 2:

[0066] Table 2 Performance test results of flame-retardant materials prepared in Examples 4-8

[0067]

[0068] As shown in Table 2, the mechanical properties of the flame-retardant material obtained by adding aminochlorobenzenesulfonamide compound to antimony trioxide are better.

[0069] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A flame-retardant material, characterized in that, The raw materials include the following components by weight: 40-85 parts nylon, 5-20 parts aluminum diisobutylphosphite, 5-20 parts brominated polystyrene, 1-3 parts antimony trioxide, 0-35 parts fiber, and 0.2-0.5 parts antioxidant; The antimony trioxide is composed of cubic antimony trioxide and orthorhombic antimony trioxide; The antimony trioxide is an aminochlorobenzenesulfonamide compound complex antimony trioxide; The aminochlorobenzenesulfonamide compound in the antimony trioxide compound includes one or two of 2-amino-4-chloro-5-methylbenzenesulfonamide and 4-amino-3-chlorobenzenesulfonamide.

2. The flame-retardant material according to claim 1, characterized in that, The mass ratio of the cubic antimony trioxide to the orthorhombic antimony trioxide is 1:2~3.

3. The flame-retardant material according to claim 1, characterized in that, The nylon includes one or both of nylon 6 and nylon 66.

4. The flame-retardant material according to claim 1, characterized in that, The antioxidant includes one or more of antioxidant 1010, antioxidant 168, and antioxidant 1076.

5. The flame-retardant material according to claim 1, characterized in that, When the fiber is not zero, the fiber includes one or more of glass fiber, carbon fiber, and aramid fiber.

6. The flame-retardant material according to claim 1, characterized in that, The raw materials for the aminochlorobenzenesulfonamide compound-antimony trioxide composite include an aminochlorobenzenesulfonamide compound and antimony trioxide in a mass ratio of 2~3:

30.

7. A method for preparing a flame-retardant material according to any one of claims 1 to 6, characterized in that, The process includes the following steps: weighing the raw materials, mixing them evenly, and then extruding and granulating them to obtain the flame-retardant material.

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