Nylon, anti-melting droplet flame retardant material containing the nylon and preparation method thereof

The nylon material produced by copolymer lactam and silicone monomers solved the problem of insufficient anti-droplet performance of existing nylon, achieved good anti-droplet and flame retardant properties of the material, and simplified the preparation process.

CN116987263BActive Publication Date: 2025-03-04INST OF CHEM CHINESE ACAD OF SCI
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Patent Information

Application Number
CN202210444937.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-04-26
Publication Date
2025-03-04
Estimated Expiration
2042-04-26

AI Technical Summary

Technical Problem

Existing nylon materials have shortcomings in their drip resistance, which may cause fire or scalds.

Method used

A nylon material is copolymerized by copolymerizing lactam and silicone monomers as polymeric monomers, which contains specific silicon structural bonds, improves the anti-droplet properties, and enhances the flame retardancy of the material by adding phosphorus-containing monomers with flame retardant properties.

Benefits of technology

It achieves good drop resistance and flame retardancy of nylon materials, simplifies the preparation process, reduces costs, and is suitable for large-scale production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to a nylon, an anti-melting drop flame retardant material containing the nylon and a preparation method, wherein the nylon comprises the following structure, wherein m is an integer selected from 5 to 11; y and z are both integers, y≥1, z≥1; R1 is phenyl, tolyl, 3-(N-cyclohexylamino)propyl, 3-cyanopropyl, aniline methyl, phenyl isobutyl, amino-(C3-C6)alkyl, phenyl-(C3-C6)alkyl or (5-6 yuan)cycloalkyl-(C3-C6)alkyl, and R2 is methyl, ethyl or phenyl. The nylon of one embodiment of the present invention is applied to flame retardant materials with good anti-melting drop performance.
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Description

Technical Field

[0001] The invention relates to nylon, in particular to nylon with good anti-melting droplet performance and materials thereof. Background Art

[0002] Nylon is widely used in various fields due to its excellent performance. However, nylon itself is not flame retardant, which may cause or aggravate fire. Therefore, how to prepare nylon with good flame retardant properties through modification has always been a concern of industry personnel. Although copolymer flame retardant nylon has been prepared, most copolymer flame retardant nylons have poor flame retardant dripping and anti-melt dripping properties. Melt dripping not only has the risk of ignition, but may also cause burns.

[0003] Some nylon anti-drip processes or products disclosed in the prior art have poor anti-drip effects, complex processes, or affect the flame retardant properties of nylon, and cannot effectively solve the anti-drip problem. For example, patent application CN112239601A obtains anti-drip nylon material by blending, and its anti-drip agent has the characteristics of surface migration and instability. Patent application CN113336993A discloses making nylon material flame retardant by surface coating, and its post-processing process is complicated, and can only be flame retardant for simple immersible structures. After treatment, the flame retardant performance and anti-drip effect are poor; in addition, the coating is flame retardant only on the surface, and once the epidermis falls off or the material is damaged, it will not have a flame retardant effect. Summary of the invention

[0004] In view of the above analysis, one embodiment of the present invention is to provide a nylon to solve the problem of poor anti-dripping performance of existing nylon.

[0005] In a first aspect, an embodiment of the present invention provides a nylon comprising the following structure:

[0006]

[0007] Wherein, m is an integer selected from 5 to 11; y and z are both integers, y≥1, z≥1; R1 is phenyl, tolyl, 3-(N-cyclohexylamino)propyl, 3-cyanopropyl, anilinomethyl, phenylisobutyl, amino-(C3~C6)alkyl, phenyl-(C3~C6)alkyl or (5~6-membered)cycloalkyl-(C3~C6)alkyl, and R2 is methyl, ethyl or phenyl.

[0008] In a second aspect, an embodiment of the present invention provides a nylon obtained by copolymerization of polymerized monomers, wherein the polymerized monomers include lactam and organosilicon monomers, and the organosilicon monomers include compounds of the following formula:

[0009]

[0010] Among them, R1 is phenyl, tolyl, 3-(N-cyclohexylamino)propyl, 3-cyanopropyl, aniline methyl, phenyl isobutyl, amino-(C3~C6)alkyl, phenyl-(C3~C6)alkyl or (5~6-membered)cycloalkyl-(C3~C6)alkyl, R2 is methyl, ethyl or phenyl, and R3 and R4 are each independently selected from methyl, ethyl or hydrogen.

[0011] According to one embodiment of the present invention, the organosilicon monomer is selected from one or more of the following compounds:

[0012]

[0013]

[0014] According to one embodiment of the present invention, the ratio of the mass m1 of the lactam to the mass m2 of the silicone monomer is m1:m2=100:(1-5).

[0015] According to one embodiment of the present invention, the lactam comprises caprolactam and / or laurolactam; and / or,

[0016] The polymerizable monomers also include phosphorus-containing monomers having flame retardant properties.

[0017] According to one embodiment of the present invention, the mass ratio of the lactam to the phosphorus-containing monomer is 100:(4-10);

[0018] According to one embodiment of the present invention, the intrinsic viscosity of the nylon is 1.8 to 3.0, and further is 2.0 to 2.8; the limiting oxygen index is 28 or more, and further is 28 to 35.

[0019] In a third aspect, an embodiment of the present invention provides a method for preparing the above-mentioned nylon, comprising mixing a polymerization monomer and a catalyst and reacting them to obtain the nylon;

[0020] Wherein, the polymerizable monomers include lactam and organosilicon monomers, and the organosilicon monomers include compounds of the following formula:

[0021]

[0022] R1 is phenyl, tolyl, 3-(N-cyclohexylamino)propyl, 3-cyanopropyl, aniline methyl, phenyl isobutyl, amino-(C3~C6)alkyl, phenyl-(C3~C6)alkyl or (5~6 membered)cycloalkyl-(C3~C6)alkyl; R2 is methyl, ethyl or phenyl; R3 and R4 are each independently selected from methyl, ethyl or hydrogen.

[0023] According to one embodiment of the present invention, the reaction process of the reaction includes: raising the temperature of the reaction system from room temperature to 220-250°C, starting the pressure-maintaining reaction for 1.5-8 hours after the system pressure reaches 1.8-3MPa, then releasing the system to normal pressure, and reacting at normal pressure for 1-8 hours after the system temperature reaches 240-320°C.

[0024] In a fourth aspect, an embodiment of the present invention provides an anti-drip flame retardant material, comprising the above-mentioned nylon and an additive, wherein the additive comprises a flame retardant.

[0025] Compared with the prior art, the present invention can achieve at least one of the following beneficial effects:

[0026] 1. The nylon according to one embodiment of the present invention has good anti-dripping performance when used in flame retardant materials.

[0027] 2. The anti-melt-dripping flame-retardant material of one embodiment of the present invention has good flame retardancy and anti-melt-dripping properties.

[0028] 3. The preparation method of the nylon / anti-drip flame retardant material according to one embodiment of the present invention has a simple process, shortens the process, reduces the cost, and is suitable for large-scale production.

[0029] In the present invention, the above-mentioned technical solutions can also be combined with each other to achieve more preferred combination solutions. Other features and advantages of the present invention will be described in the subsequent description, and some advantages can become obvious from the description, or can be understood by practicing the present invention. The purpose and other advantages of the present invention can be achieved and obtained through the contents particularly pointed out in the description. DETAILED DESCRIPTION

[0030] The preferred embodiments of the present invention are described in detail below, which are used to illustrate the principles of the present invention but are not used to limit the scope of the present invention.

[0031] An embodiment of the present invention provides a nylon comprising the following structure:

[0032]

[0033] Wherein, m is an integer selected from 5 to 11; y and z are both integers, representing the number of repeating units, y≥1, z≥1; R1 is phenyl, tolyl (CH3-Ar-), 3-(N-cyclohexylamino)propyl (C6H 11 -NH-(CH2)3-), 3-cyanopropyl (CN-(CH2)3-), aniline methyl (Ar-NH-CH2-) or phenyl isobutyl (Ar-C(CH3)2-CH2-); R2 is methyl, ethyl or phenyl. Wherein, Ar- in the above brackets represents phenyl.

[0034] The nylon of one embodiment of the present invention not only solves the problem of poor stability of anti-dripping agents in existing flame retardant materials by bonding a specific silicon-containing structure to a polymer chain, but also greatly improves the anti-dripping performance of the material, so that the nylon can exhibit excellent anti-dripping properties with only a small amount of silicon structure; in addition, the preparation process of the nylon is simple, the process is shortened, the cost is reduced, and it is suitable for large-scale production.

[0035] In one embodiment, the value of m can be 6, 7, 8, 9, 10, 11 or 12.

[0036] In one embodiment, R1 is phenyl or tolyl, and further, the tolyl may be p-tolyl; R2 is methyl or phenyl.

[0037] In one embodiment, the intrinsic viscosity of nylon is 1.8 to 3.0, such as 2.0, 2.2, 2.3, 2.5, 2.6, or 2.8; further, it may be 2.2 to 2.8.

[0038] In one embodiment, the structure of Formula I represents a partial segment of a polymer molecule, and does not represent the structure of the entire molecule.

[0039] The nylon of one embodiment of the present invention comprises a polyamide molecule and a modified polyamide molecule, wherein the polyamide molecule is composed of a polyamide structure as shown below; the modified polyamide molecule is composed of a polyamide structure and a silicon-containing structure interlaced, for example, it may comprise a structure as shown in Formula I;

[0040]

[0041] Here, x can be an integer greater than or equal to 2.

[0042] The nylon according to one embodiment of the present invention can be prepared by copolymerization of polymerizable monomers, wherein the polymerizable monomers include lactam and organosilicon monomers, and the organosilicon monomers include compounds of the following formula:

[0043]

[0044] Wherein, R1 is phenyl, tolyl, 3-(N-cyclohexylamino)propyl, 3-cyanopropyl, anilinemethyl or phenylisobutyl; R2 is methyl, ethyl or phenyl; R3 and R4 are each independently selected from methyl, ethyl or hydrogen.

[0045] In one embodiment, the organosilicon monomer may be one or more of the following compounds:

[0046]

[0047]

[0048]

[0049] In one embodiment, the presence of the organosilicon monomer during the copolymerization process causes it to participate in the polymerization reaction and insert into the polyamide chain. The reaction that occurs can be shown as follows:

[0050]

[0051] Among them, the above reaction formula is only an example and not a limitation of the polymerization product. If the content of the silicone monomer is high, two or more silicon-oxygen structures (-O-Si(R1R2)-O-) in the above reaction formula will be inserted into one polyamide molecular chain to form a modified polyamide molecule; if the content of the silicone monomer is low, one silicon-oxygen structure will be inserted into one polyamide molecular chain, or the silicon-oxygen structure will be inserted only into part of the polyamide molecular chain, that is, the formed nylon contains both polyamide molecules and the aforementioned modified polyamide molecules.

[0052] In one embodiment, the ratio of the mass m1 of the lactam to the mass m2 of the silicone monomer in the polymerized monomer is m1:m2=100:(1-5), for example, 100:2, 100:3, 100:4.

[0053] In one embodiment, the lactam may be one or both of caprolactam and laurolactam.

[0054] In one embodiment, the polymerized monomer further comprises a phosphorus-containing monomer having flame retardant properties, and after copolymerization, the anti-drip flame retardant nylon is obtained; the limiting oxygen index of the anti-drip flame retardant nylon may be greater than 28, further 28 to 35, for example 29, 30, 31, 32, 33, 34.

[0055] In one embodiment, the phosphorus-containing monomer may be, for example, a DOPO-based reactive phosphorus flame retardant (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), 2-hydroxyethylphenylphosphine or bis(p-hydroxyphenyl)phenylphosphine oxide, 10-(2,5-dicarboxyphenoxy)-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide (DOPODP), 2-(dimethyl phosphate)-4,6-(2′-carboxyethylphenylphosphinic acid)-s-triazine (DPPATPO), 2-carboxyethylphenylphosphinic acid (CEPPA), [(6-oxo-6H-dibenzo[c,e][1,2]oxaphosphorin-6-yl)methyl ] succinic acid (DDP), 2,2-bis((4-phenoxyphenylphosphine oxide)-p-aminobenzoic acid) propane (BPOAP), 2-(dimethyl phosphate)-4,6-(p-aminobenzoic acid)-s-triazine (DPTPO), di-1-oxophospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane-1-phenyl-4-oxophosphine (BPEPA), 2-(dimethyl phosphate)-4,6-(2-hydroxypropionic acid)-s-triazine, 4-(2-(((carboxyethyl)(phenyl)phosphine oxide)oxy)ethoxy)-4-oxohexanoic acid (CPPOA), bis(3-aminophenyl)phenylphosphine oxide (BAPPO).

[0056] In one embodiment, the mass ratio of lactam to phosphorus-containing monomer may be 100:(4-10), for example, 100:5, 100:6, or 100:8.

[0057] In one embodiment, a catalyst can be added to the reaction system to accelerate the copolymerization reaction of the polymerization monomer; further, the catalyst can be hypophosphite, organic phosphoric acid, or a dibasic acid, and the ratio of the mass of the lactam in the polymerization monomer to the mass of the catalyst can be 100:(0.05-1), for example, 100:0.2, 100:0.5, 100:0.6, or 100:0.8.

[0058] In one embodiment, an antioxidant may be added to the reaction system. The antioxidant may be one or more of antioxidant 168, antioxidant 1098, antioxidant 1010, and antioxidant 626.

[0059] In one embodiment, the polymerization reaction system may include the following components: 100 parts by mass of lactam, 10-50 parts by mass of water, 4-10 parts by mass of phosphorus-containing monomers, 1-5 parts by mass of organosilicon monomers, 0.05-1 parts by mass of catalysts, and 0.1-0.5 parts by mass of antioxidants.

[0060] In one embodiment, before the copolymerization reaction, the phosphorus-containing monomer is first prepared into a flame retardant salt solution by diamine, the molar ratio of the phosphorus-containing monomer to the diamine can be 1:1 to 1:1.2, the salt-forming reaction temperature is 60 to 90°C, for example, 65°C, 70°C, 75°C, 80°C, 85°C; the reaction time can be 0.5 to 3 hours, for example, 1 hour, 2 hours, 2.5 hours; the solid content of the solution can be 30 to 80%, for example, 40%, 50%, 60%, 70%.

[0061] In one embodiment, the diamine that undergoes salt formation reaction with the phosphorus-containing monomer may be an aliphatic diamine containing 4 to 12 carbon atoms, such as one or more of butanediamine, pentamethylenediamine, hexamethylenediamine, decanediamine, and dodecanediamine.

[0062] In one embodiment, the preparation process of nylon includes: mixing a silicone monomer, a flame retardant salt solution with a lactam, water, and a catalyst into a reaction container; replacing the air in the reaction container with nitrogen, raising the temperature in the container from room temperature to 220-250°C, and starting a pressure-maintaining reaction for 1.5-8 hours after the pressure in the container reaches 1.8-3MPa, and then evenly releasing it to normal pressure. After the temperature in the reaction container reaches 240-320°C, react at normal pressure for 1-8 hours, evacuate for 30-60 minutes, and discharge the material after determining that the torque no longer increases or reaches the corresponding viscosity.

[0063] In one embodiment, in the preparation process of nylon, after the air in the reaction container is replaced with nitrogen, the temperature in the container can be raised to 230°C, 235°C or 240°C; after the pressure in the container reaches 2MPa, 2.2MPa, 2.5MPa or 2.8MPa, the pressure holding reaction is started, and the pressure holding reaction time can be 2 hours, 3 hours, 4 hours, 5 hours, 6 hours or 7 hours, and then the pressure is evenly released to normal pressure. After the temperature in the reaction container reaches 260°C, 270°C, 280°C, 290°C, 300°C or 310°C, the reaction is carried out at normal pressure for 2 hours, 3 hours, 4 hours, 5 hours, 6 hours or 7 hours.

[0064] An embodiment of the present invention further provides an anti-drip flame retardant material, comprising the above-mentioned nylon and additives.

[0065] In one embodiment, the polymerized monomer of nylon includes a phosphorus-containing monomer having flame retardant properties, and the anti-drip flame retardant material does not need to be additionally added with a flame retardant.

[0066] In one embodiment, the polymerized monomer of nylon does not include a monomer having flame retardant properties, and the additive of the anti-drip flame retardant material includes a flame retardant, which can be an existing flame retardant used for blending and addition.

[0067] In one embodiment, the intrinsic viscosity of the anti-drip flame retardant material may be 1.8 to 3.0, such as 2.0, 2.2, 2.3, 2.4, 2.5, 2.6, or 2.8; further, it may be 2.2 to 2.8.

[0068] In one embodiment, the limiting oxygen index of the anti-drip flame retardant material is 28 or more, and further is 28-35, for example, 29, 30, 31, 32, 33, 34.

[0069] The nylon / anti-drip flame retardant material according to one embodiment of the present invention has good flame retardancy and anti-drip properties and can maintain excellent mechanical properties.

[0070] The nylon / anti-drip flame retardant material of one embodiment of the present invention does not need to be compounded with a flame retardant (phosphorus-containing monomer), requires fewer types of flame retardants to be added, has a simple reaction process, and can be prepared in a one-step reactor.

[0071] The nylon / anti-drip flame retardant material of one embodiment of the present invention has a simple preparation process, a short process time, reduced costs, and is suitable for large-scale production.

[0072] The preparation of the anti-drip flame-retardant nylon material according to one embodiment of the present invention is further described below in conjunction with specific examples. The intrinsic viscosity is measured with reference to the standard GBT 12006.1-2009, the limiting oxygen index is measured with reference to the standard GB-2406-2009, the flame retardant grade is measured with reference to the standard GBT2408-2008, and the tensile strength is measured with reference to the standard GB / T 1040-2006.

[0073] Example 1

[0074] Preparation of flame retardant salt solution

[0075] 150 g of DOPO phosphorus-containing monomer flame retardant, 70 g of hexamethylenediamine and 200 g of water were mixed and reacted at 60° C. for 1 hour to prepare a flame retardant salt solution.

[0076] Preparation of nylon materials

[0077] The flame retardant salt solution, 100g of diphenylsilanediol, 2g of hypophosphite and 20g of antioxidant 168 prepared above are mixed and put into a reactor, stirred with a magnetic stirrer for 10 minutes, and then mixed with 2kg of caprolactam and sealed; the reactor temperature is controlled to rise from room temperature to 220°C, and the pressure in the reactor is kept at 2.2MPa for 2 hours; then, the mixture is evenly vented to normal pressure, and the reaction is carried out at normal pressure for 120 minutes after the reactor temperature reaches 240-260°C, and finally evacuated to absolute pressure for 60 minutes. After the torque (Torque) reaches 1 and no longer rises, the material is discharged to obtain an anti-drip flame-retardant nylon material.

[0078] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0079] Example 1-1

[0080] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer diphenylsilanediol used is 20 g.

[0081] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0082] Example 1-2

[0083] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer diphenylsilanediol used is 60 g.

[0084] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0085] Examples 1-3

[0086] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer diphenylsilanediol used is 200 g.

[0087] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0088] Example 2

[0089] This embodiment adopts the same raw materials and steps as those in Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is p-toluene dimethoxysilane.

[0090] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0091] Example 2-1

[0092] This embodiment adopts the same raw materials and steps as those of Embodiment 2 to prepare the anti-drip flame-retardant nylon material, with the only difference being that the mass of the organic silicon monomer p-toluenemethyldimethoxysilane used is 20 g.

[0093] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0094] Example 3

[0095] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is methylphenyldimethoxysilane.

[0096] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0097] Example 3-1

[0098] This embodiment adopts the same raw materials and steps as those of Embodiment 3 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer methylphenyldimethoxysilane used is 20 g.

[0099] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0100] Example 4

[0101] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is diethoxymethylphenylsilane.

[0102] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0103] Example 4-1

[0104] This embodiment adopts the same raw materials and steps as those of embodiment 4 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer diethoxymethylphenylsilane used is 20 g.

[0105] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0106] Example 5

[0107] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is diphenyldimethoxysilane.

[0108] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0109] Example 5-1

[0110] This embodiment adopts the same raw materials and steps as those of Embodiment 5 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer diphenyldimethoxysilane used is 20 g.

[0111] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0112] Example 6

[0113] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is 3-(N-cyclohexylamino)propylmethyldimethoxysilane.

[0114] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0115] Example 6-1

[0116] This embodiment adopts the same raw materials and steps as those of Embodiment 6 to prepare the anti-drip flame-retardant nylon material, with the only difference being that the mass of the organic silicon monomer 3-(N-cyclohexylamino)propylmethyldimethoxysilane used is 20 g.

[0117] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0118] Example 7

[0119] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is 3-cyanopropylphenyldimethoxysilane.

[0120] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0121] Example 7-1

[0122] This embodiment adopts the same raw materials and steps as those of Embodiment 7 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer 3-cyanopropylphenyldimethoxysilane used is 20 g.

[0123] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0124] Example 8

[0125] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is anilinemethylmethyldimethoxysilane.

[0126] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0127] Example 8-1

[0128] This embodiment adopts the same raw materials and steps as those of Embodiment 8 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer anilinemethylmethyldimethoxysilane used is 20 g.

[0129] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0130] Example 9

[0131] This embodiment adopts the same raw materials and steps as those of Embodiment 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is phenyl tert-butyl methyl dimethoxy silane.

[0132] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0133] Example 9-1

[0134] This embodiment adopts the same raw materials and steps as those of Embodiment 9 to prepare the anti-drip flame-retardant nylon material, the only difference being that the mass of the organic silicon monomer phenyl tert-butyl methyl dimethoxy silane used is 20 g.

[0135] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0136] Example 10

[0137] This embodiment adopts the same raw materials and steps as those of Embodiment 1-1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the lactam used is lauryl lactam.

[0138] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0139] Comparative Example 1

[0140] This example uses the same raw materials and steps as Example 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is amino silicone oil, and its structural formula is as follows:

[0141]

[0142] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0143] Comparative Example 2

[0144] This example adopts the same raw materials and steps as Example 1 to prepare the anti-drip flame-retardant nylon material, the only difference being that the organic silicon monomer used is 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane.

[0145] The obtained anti-melt droplet flame retardant nylon material was subjected to relevant performance tests, and the specific results are shown in Table 1.

[0146] Table 1

[0147]

[0148]

[0149] As shown in Table 1, the nylon material prepared by using a specific type of organosilicon monomer in the embodiment of the present invention has good flame retardancy, excellent anti-dripping performance, and also has good mechanical properties. Although comparative examples 1 and 2 also use organosilicon monomers for polymerization, their anti-melting dripping performance is poor and still causes dripping and ignition; and the flame retardancy and tensile strength of the nylon material are also worse than those of the nylon material in the embodiment.

[0150] Further referring to the results of Examples 1 to 1-3 and Table 1, it can be seen that the nylon material of the embodiment of the present invention can show good anti-melting dripping performance when the mass ratio of nylon salt to silicone monomer is 100:1, that is, only a small amount of silicone monomer needs to be added to obtain good anti-melting dripping performance. In addition, among Examples 1 to 1-3, although the limiting oxygen index of Example 1-3 is the highest, its tensile strength is the lowest. Based on the consideration of comprehensive performance, the ratio of the mass m1 of the lactam in the polymerized monomer to the mass m2 of the silicone monomer is preferably m1:m2=100:(1~5).

[0151] Comparing the characterization results of Examples 1, 2, 3, 4, and 5, it can be seen that the nylon materials of Examples 3 and 4 have higher limiting oxygen index and tensile strength. Therefore, the organosilicon monomer is preferably methylphenyldimethoxysilane and diethoxymethylphenylsilane.

[0152] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention.

Claims

1. A nylon, characterized in that: The nylon comprises the following structure: ; wherein m is an integer selected from 5 to 11; y and z are both integers, y≥1, z≥1; R1 is phenyl, and R2 is methyl; The nylon is prepared by copolymerization of polymerized monomers, wherein the polymerized monomers include lactam and organosilicon monomers, and the structural formula of the organosilicon monomer is as follows: ; The ratio of the mass m1 of the lactam to the mass m2 of the silicone monomer is m1:m2=100:(1-5); The polymerizable monomers also include phosphorus-containing monomers having flame retardant properties; The mass ratio of the lactam to the phosphorus-containing monomer is 100:(4-10).

2. The nylon according to claim 1, characterized in that The lactam includes caprolactam and / or laurolactam.

3. The nylon according to claim 2, characterized in that: The intrinsic viscosity of the nylon is measured to be 1.8 to 3.0 according to the standard GBT 12006.1-2009; the limiting oxygen index of the nylon is measured to be above 28 according to the standard GB-2406-2009.

4. The nylon according to claim 3, characterized in that The intrinsic viscosity of the nylon is 2.0-2.8, and the limiting oxygen index of the nylon is 28-35.

5. A method for preparing nylon according to any one of claims 1 to 4, characterized in that: The method comprises mixing a polymerization monomer and a catalyst and reacting the mixture to obtain the nylon; Wherein, the polymerizable monomers include lactam and organosilicon monomers, and the structural formula of the organosilicon monomers is as follows: 。 6. The preparation method according to claim 5, characterized in that: The reaction process of the reaction comprises: raising the temperature of the reaction system from room temperature to 220-250° C., starting a pressure-maintaining reaction for 1.5-8 hours after the system pressure reaches 1.8-3 MPa, then releasing the system to normal pressure, and reacting at normal pressure for 1-8 hours after the system temperature reaches 240-320° C.

7. An anti-drip flame retardant material, characterized in that: The invention comprises the nylon according to any one of claims 1 to 4 and an additive, wherein the additive comprises a flame retardant.

Citation Information

Patent Citations

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