Flame-retardant nylon material and preparation method therefor

By compounding diisobutyl aluminum hypophosphite and brominated polystyrene flame retardant into nylon materials, flame-retardant nylon materials are prepared, solving the problems of insufficient flame retardant performance and poor mechanical properties in the existing technology, and achieving high-efficiency flame retardancy and improved mechanical properties.

WO2025241237A1PCT designated stage Publication Date: 2025-11-27HEBEI XINXINYUAN ENERGY CO LTD

Patent Information

Application Number
PCT/CN2024/099457
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-05-20
Filing Date
2024-06-15
Publication Date
2025-11-27

AI Technical Summary

Technical Problem

Existing flame retardants for nylon materials have problems with insufficient flame retardant performance and poor mechanical properties. In particular, when diethyl aluminum hypophosphite is used alone, it needs to be compounded with other additives, resulting in high cost and poor effect.

Method used

A mixture of diisobutyl aluminum hypophosphite and brominated polystyrene was used as a flame retardant and incorporated into nylon materials. Nylon flame retardant materials were prepared by extrusion granulation, and the component ratio was optimized to improve flame retardant performance and mechanical properties.

Benefits of technology

It significantly improves the flame retardant and mechanical properties of nylon materials, achieving a flame retardant rating of UL94 1.6 mm V0, a ​​10% increase in mechanical properties, a 10% decrease in density, and a 30°C increase in high-temperature resistance, while also solving the problem of poor coloring of bromine flame retardants.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

A flame-retardant nylon material and a preparation method therefor. The components of a flame retardant in the flame-retardant nylon material comprise a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene. The technical solution overcomes the problems of insufficient flame retardant properties and poor mechanical properties of existing flame retardants when added to plastics in the prior art.
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Description

Nylon flame-retardant material and preparation method thereof TECHNICAL FIELD

[0001] The present application relates to the technical field of flame-retardant materials, in particular to a nylon flame-retardant material and a preparation method thereof. BACKGROUND

[0002] The halogen-free flame retardant added in engineering plastics such as nylon 6 and nylon 66 mainly includes microencapsulated red phosphorus masterbatch, aluminum (magnesium) hydroxide, melamine cyanurate and phosphorus-based flame retardant.

[0003] Among them, the phosphorus-based flame retardant has the advantages of environmental protection, low smoke, non-toxic, etc., and the application in engineering plastics such as nylon is mainly aluminum diethyl phosphite (ADP), but aluminum diethyl phosphite cannot be used alone, and the existing main MPP (melamine polyphosphate), MCA (melamine cyanurate), aluminum phosphite and other flame retardants are compounded and used, and various other additives need to be added, and at present, when the flame retardant is used, there are problems such as large addition amount, high cost, insufficient flame retardant performance and mechanical property reduction when added to engineering plastics such as nylon.

[0004] SUMMARY

[0005] The present application provides a nylon flame-retardant material and a preparation method thereof, which solves the problems of insufficient flame-retardant performance and poor mechanical property of the existing flame retardant added in plastics in the related art.

[0006] The technical scheme of the present application is as follows:

[0007] The present application provides a flame retardant containing brominated polystyrene, characterized in that the components include a mixture of diisobutyl aluminum phosphite and brominated polystyrene.

[0008] As a further technical scheme, the mass ratio of diisobutyl aluminum phosphite and brominated polystyrene is 1:0.1-2.

[0009] The present application also provides a nylon flame-retardant material, which includes a base material, an antioxidant, a filler and the flame retardant; the base material includes one or both of nylon 6 and nylon 66.

[0010] As a further technical scheme, when the base material is nylon 6, the nylon flame-retardant material includes the following components by weight: 45-65 parts of nylon 6, 10-28 parts of flame retardant, 0.2-0.5 parts of antioxidant and 25-35 parts of filler.

[0011] As a further technical scheme, the mass ratio of diisobutyl aluminum phosphite and brominated polystyrene in the flame retardant is 1:0.2-1.5.

[0012] In the application, when the mass ratio of aluminum diisobutyl phosphinate and brominated polystyrene is 1:0.2-1.5, the mechanical property of the nylon flame-retardant material is further improved under the condition of ensuring the flame-retardant property.

[0013] As a further technical solution, the mass ratio of aluminum diisobutyl phosphinate and brominated polystyrene in the flame retardant is 1:0.5-1.

[0014] In the application, when the mass ratio of aluminum diisobutyl phosphinate and brominated polystyrene is 1:0.5-1, the mechanical property of the nylon flame-retardant material is further improved under the condition of ensuring the flame-retardant property.

[0015] As a further technical solution, when the base material is nylon 66, the nylon flame-retardant material comprises the following components by weight: 45-65 parts of nylon 66, 5-22 parts of flame retardant, 0.2-0.5 parts of antioxidant, and 25-35 parts of filler.

[0016] As a further technical solution, the component further comprises a styrene-methyl methacrylate copolymer.

[0017] As a further technical solution, the nylon flame-retardant material specifically comprises 6-8 parts of styrene-methyl methacrylate copolymer by weight.

[0018] In the application, the addition of styrene-methyl methacrylate copolymer in the nylon flame-retardant material can promote the dispersion of the flame retardant in the nylon material, and further improve the mechanical property of the nylon flame-retardant material.

[0019] As a further technical solution, the antioxidant is one or more of antioxidant 626, antioxidant BHT, antioxidant 1010, antioxidant 1076, and antioxidant 168; and the filler comprises one or more of glass fiber, basalt fiber, and carbon fiber.

[0020] The application further provides a preparation method of the nylon flame-retardant material, comprising the following steps: mixing the components of the nylon flame-retardant material, and then extruding and granulating to obtain the nylon flame-retardant material.

[0021] The working principle and beneficial effects of the application are as follows:

[0022] 1. In the application, the flame retardant is compounded by brominated polystyrene (BPS) and aluminum diisobutyl phosphinate, and the synergistic flame retardant can completely replace the existing bromine+antimony flame retardant, has the characteristics of low cost, small amount, and excellent flame-retardant effect.

[0023] 2、The application adds the flame retardant of the mixture of brominated polystyrene and aluminum diisobutyl phosphinate into the formula with nylon as the matrix, the flame retardant can be inter-dissolved with the nylon matrix as the organic matter without the segregation phenomenon, the flame retardant performance and the mechanical property of the nylon material are improved obviously, wherein the flame retardant level of the nylon flame retardant material can reach UL94 1.6 millimeter V0, the mechanical property can be improved by 10%, in addition, the density of the nylon flame retardant material is reduced by 10%, the high temperature resistance is improved by 30 DEG C, in addition, the problem that the bromine flame retardant bright product is not good coloring is solved. DETAILED DESCRIPTION

[0024] The technical solutions in the embodiments of the application will be clearly and completely described below with reference to the embodiments of the application. Obviously, the described embodiments are only part of the embodiments of the application, rather than all the embodiments of the application. Based on the embodiments of the application, all other embodiments obtained by a person of ordinary skill in the art without creative work fall within the protection scope of the application.

[0025] In the following examples and comparative examples, the type of styrene-methyl methacrylate copolymer is PM-600; the type of brominated polystyrene is XZ-6700, which is purchased from Shandong Brothers Science and Technology Co., Ltd.; the type of aluminum diisobutyl phosphinate is D13 (particle size: 1-3 mm); the type of nylon 6 is YH400, which is purchased from Hunan Yuehua Chemical Co., Ltd.; the type of nylon 66 is EPR27, which is purchased from Pingdingshan Shenma Engineering Plastics Co., Ltd.

[0026] Example 1

[0027] The flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl phosphinate and brominated polystyrene with a mass ratio of 1:1;

[0028] The nylon flame retardant material comprises the following components in parts by weight: 56.7 parts of nylon 6, 16 parts of the flame retardant containing brominated polystyrene, 0.3 parts of antioxidant 626, and 30 parts of glass fiber.

[0029] The preparation method of the nylon flame retardant material comprises the following steps: mixing the components of the nylon flame retardant material, and then extruding and granulating to obtain the nylon flame retardant material.

[0030] Example 2

[0031] The flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl phosphinate and brominated polystyrene with a mass ratio of 1:1;

[0032] The nylon flame retardant material comprises the following components in parts by weight: 45 parts of nylon 6, 10 parts of the flame retardant containing brominated polystyrene, 0.2 parts of antioxidant 626, and 25 parts of glass fiber.

[0033] The preparation method of the nylon flame-retardant material comprises the following steps: mixing the components of the nylon flame-retardant material, and then extruding and granulating to obtain the nylon flame-retardant material.

[0034] Example 3

[0035] The flame retardant containing brominated polystyrene comprises components including a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene with a mass ratio of 1:1;

[0036] The nylon flame-retardant material comprises the following components by weight: 65 parts of nylon 6, 28 parts of the flame retardant containing brominated polystyrene, 0.5 parts of antioxidant 626, and 35 parts of glass fiber;

[0037] The preparation method of the nylon flame-retardant material comprises the following steps: mixing the components of the nylon flame-retardant material, and then extruding and granulating to obtain the nylon flame-retardant material.

[0038] Example 4

[0039] The flame retardant containing brominated polystyrene comprises components including a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene with a mass ratio of 1:1;

[0040] The nylon flame-retardant material comprises the following components by weight: 59.6 parts of nylon 66, 14 parts of the flame retardant, 0.4 parts of antioxidant 626, and 30 parts of glass fiber;

[0041] The preparation method of the nylon flame-retardant material comprises the following steps: mixing the components of the nylon flame-retardant material, and then extruding and granulating to obtain the nylon flame-retardant material.

[0042] Example 5

[0043] The flame retardant containing brominated polystyrene comprises components including a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene with a mass ratio of 1:1;

[0044] The nylon flame-retardant material comprises the following components by weight: 45 parts of nylon 66, 5 parts of the flame retardant, 0.2 parts of antioxidant 626, and 25 parts of glass fiber;

[0045] The preparation method of the nylon flame-retardant material comprises the following steps: mixing the components of the nylon flame-retardant material, and then extruding and granulating to obtain the nylon flame-retardant material.

[0046] Example 6

[0047] The flame retardant containing brominated polystyrene comprises components including a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene with a mass ratio of 1:1;

[0048] The nylon flame retardant material comprises the following components by weight: nylon 66 65 parts, flame retardant 22 parts, antioxidant 626 0.5 parts, glass fiber 35 parts.

[0049] The method for preparing the nylon flame retardant material comprises the following steps: mixing the components of the nylon flame retardant material, and then extruding and granulating to obtain the nylon flame retardant material.

[0050] Example 7

[0051] The difference between this example and Example 1 is only that the flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene in a mass ratio of 1:0.1.

[0052] Example 8

[0053] The difference between this example and Example 1 is only that the flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene in a mass ratio of 1:2.

[0054] Example 9

[0055] The difference between this example and Example 1 is only that the flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene in a mass ratio of 1:0.2.

[0056] Example 10

[0057] The difference between this example and Example 1 is only that the flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene in a mass ratio of 1:1.5.

[0058] Example 11

[0059] The difference between this example and Example 1 is only that the flame retardant containing brominated polystyrene comprises a mixture of aluminum diisobutyl hypophosphite and brominated polystyrene in a mass ratio of 1:0.5.

[0060] Example 12

[0061] The difference between this example and Example 1 is only that the nylon flame retardant material comprises the following components by weight: nylon 6 56.7 parts, flame retardant containing brominated polystyrene 16 parts, antioxidant 626 0.3 parts, glass fiber 30 parts, and styrene-methyl methacrylate copolymer 8 parts.

[0062] Example 13

[0063] The difference between this example and Example 4 is that the nylon flame retardant material comprises the following components by weight: nylon 66 59.6 parts, flame retardant 14 parts, antioxidant 626 0.4 parts, glass fiber 30 parts, styrene-methyl methacrylate copolymer 6 parts.

[0064] Comparative Example 1

[0065] The difference between this comparative example and Example 1 is that the brominated polystyrene-containing flame retardant comprises aluminum diisobutylphosphinate.

[0066] Comparative Example 2

[0067] The difference between this comparative example and Example 1 is that the brominated polystyrene-containing flame retardant comprises brominated polystyrene.

[0068] Comparative Example 3

[0069] The difference between this comparative example and Example 1 is that the brominated polystyrene-containing flame retardant comprises a mixture of aluminum diisobutylphosphinate and brominated polystyrene in a mass ratio of 1:3.

[0070] Comparative Example 4

[0071] The difference between this comparative example and Example 4 is that the brominated polystyrene-containing flame retardant comprises aluminum diisobutylphosphinate.

[0072] Comparative Example 5

[0073] The difference between this comparative example and Example 4 is that the brominated polystyrene-containing flame retardant comprises brominated polystyrene.

[0074] Comparative Example 6

[0075] The difference between this comparative example and Example 4 is that the brominated polystyrene-containing flame retardant comprises a mixture of aluminum diisobutylphosphinate and brominated polystyrene in a mass ratio of 1:3.

[0076] Comparative Example 7

[0077] The difference between this comparative example and Example 1 is that the nylon flame retardant material comprises the following components by weight: nylon 6 56.7 parts, antioxidant 626 0.3 parts, glass fiber 30 parts, styrene-methyl methacrylate copolymer 8 parts.

[0078] The performance tests were carried out on the nylon flame retardant materials prepared in Examples 1-6 and Comparative Examples 1-6, respectively. Each test sample was tested in triplicate, and the average value was taken. The test results are shown in Tables 1-2 below.

[0079] Table 1 Performance test results

[0080] Table 2 Performance test results

[0081] It is found by comparing the data of Examples 1-6 and Comparative Examples 1-6 that, compared with Comparative Examples 1-3, the flame retardant grades of the flame retardant materials of nylon 6 prepared in Examples 1-3 are higher, and the mechanical properties such as tensile strength and impact strength are more excellent; compared with Comparative Examples 4-6, the flame retardant grades of the flame retardant materials of nylon 66 prepared in Examples 4-6 are higher, and the mechanical properties such as tensile strength and impact strength are higher; it is indicated that the brominated polystyrene and aluminum diisobutyl hypophosphite are compounded and added into the formula with nylon as the matrix to synergistically flame retard, which significantly improves the flame retardant properties and mechanical properties of the nylon flame retardant materials.

[0082] The performance of the nylon flame retardant materials prepared in Examples 7-11 is respectively tested, and the test results are shown in Table 3.

[0083] Table 3 Performance test results

[0084] It is found by comparing the data of Examples 7-10 that, compared with Examples 7-8, the impact strength of the nylon 6 flame retardant materials prepared in Examples 9-10 is higher, which indicates that when the mass ratio of aluminum diisobutyl hypophosphite to brominated polystyrene is 1:0.2-1.5, the mechanical properties of the nylon flame retardant materials are further improved.

[0085] It is found by comparing the data of Examples 1, 7-11 that, compared with Examples 7-10, the impact strength of the nylon 6 flame retardant materials prepared in Examples 1, 11 is higher, which indicates that when the mass ratio of aluminum diisobutyl hypophosphite to brominated polystyrene is 1:0.5-1, the mechanical properties of the nylon flame retardant materials are further improved.

[0086] The impact performance of the nylon flame retardant materials prepared in Examples 12-13 and Comparative Example 7 is respectively tested, and the test results are shown in Table 4.

[0087] Table 4 Performance test results

[0088] It is found by comparing the data of Examples 1, 4, 12-13 and Comparative Example 7 that, compared with Examples 1, 4, the impact strength of the nylon flame retardant materials prepared in Examples 12-13 is higher, and compared with Comparative Example 7, the impact strength of the nylon flame retardant material prepared in Example 12 is higher, which indicates that the styrene-methyl methacrylate copolymer is added in the nylon flame retardant material to cooperate with the flame retardant, which can further improve the mechanical properties of the nylon flame retardant material.

[0089] The above merely preferred embodiments of the present application are not used to limit the present application, any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A flame retardant nylon material characterized in that, The components include a base material, an antioxidant, a filler, and a flame retardant; the base material includes one or both of nylon 6 and nylon 66; The components of the flame retardant include a mixture of aluminum diisobutyl phosphinate and brominated polystyrene; When the base material is nylon 6, the nylon flame-retardant material includes the following components by weight: 45-65 parts of nylon 6, 10-28 parts of the flame retardant, 0.2-0.5 parts of the antioxidant, and 25-35 parts of the filler. The components of the nylon flame-retardant material further include a styrene-methyl methacrylate copolymer.

2. A flame retardant nylon material according to claim 1, wherein The mass ratio of aluminum diisobutyl phosphinate to brominated polystyrene in the flame retardant is 1:0.1-2.

3. A flame retardant nylon material according to claim 2, wherein The mass ratio of aluminum diisobutyl phosphinate to brominated polystyrene in the flame retardant is 1:0.2-1.

5.

4. A flame retardant nylon material according to claim 3, wherein The mass ratio of aluminum diisobutyl phosphinate to brominated polystyrene in the flame retardant is 1:0.5-1.

5. The flame retardant nylon material of claim 1, wherein When the base material is nylon 66, the nylon flame-retardant material includes the following components by weight: 45-65 parts of nylon 66, 5-22 parts of the flame retardant, 0.2-0.5 parts of the antioxidant, and 25-35 parts of the filler.

6. The nylon flame retardant material of claim 1, wherein The antioxidant is one or more of antioxidant 626, antioxidant BHT, antioxidant 1010, antioxidant 1076, and antioxidant 168; the filler includes one or more of glass fiber, basalt fiber, and carbon fiber.

7. The method for preparing a flame-retardant nylon material according to any one of claims 1 to 6, characterized in that, The method includes the following steps: After the components of the nylon flame-retardant material are mixed, they are extruded and granulated to obtain the nylon flame-retardant material.

Citation Information

Patent Citations

  • Phosphorus-bromine compound reinforced flame-retardant nylon 66 composite material and preparation method thereof

    CN108997747A

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    CN118206871A

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