A multilayer composite fabric and a method for preparing the same by irradiation

By using a multi-layer composite fabric structure and irradiation vulcanization technology, the problem of easy peeling of intumescent flame retardant materials in the rubber matrix is ​​solved, achieving a soft and highly efficient flame retardant effect.

CN116852819BActive Publication Date: 2025-11-21SICHUAN FIRE RES INST OF MEM
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Patent Information

Application Number
CN202310840066.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-10
Publication Date
2025-11-21
Estimated Expiration
2043-07-10

AI Technical Summary

Technical Problem

Existing intumescent flame retardant materials are easily peeled off from the rubber matrix, affecting their flexibility and flame retardant effect.

Method used

The fabric adopts a multi-layer composite structure, including fluororubber sheets, flame-retardant fluorosilicone rubber sheets and fabric layers. Vermiculite powder and expandable graphite powder are combined with fluorosilicone rubber through radiation vulcanization technology to form a stable structure.

Benefits of technology

While maintaining flexibility, it improves flame retardant properties, prevents the expansion material from delaminating from the matrix, and enhances overall stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of multilayer composite fabric and its irradiation preparation method, it is related to fireproof material field.The application is made by fluorine rubber sheet, flame-retardant fluorosilicone rubber sheet, fabric layer and neoprene sheet sequentially adheres, the fluorine rubber sheet is as external fabric, the neoprene sheet is as internal fabric, the fluorine rubber sheet and the flame-retardant fluorosilicone rubber sheet are heat-pressed and adhered to form external layer, the edge of the external layer is heat-pressed and fused with the edge of the neoprene sheet connection;The flame-retardant fluorosilicone rubber sheet is prepared under irradiation condition vulcanization;To achieve the purpose of providing a kind of soft and good flame-retardant fabric.
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Description

Technical Field

[0001] This invention relates to the field of fire-resistant materials, specifically to a multi-layer composite fabric and its irradiation preparation method. Background Technology

[0002] Flame-retardant rubber refers to rubber that possesses both flame-retardant and flame-resistance properties. Rubber is an organic flammable material, posing a safety hazard. Therefore, rubber conveyor belts used in mines and various rubber products used in vehicles and ships are required to have flame-retardant and flame-resistance properties. Adding flame retardants is a method to improve the flame-retardancy of rubber. Commonly used flame retardants include: a combination of chlorinated paraffin and antimony trioxide, aluminum hydroxide, sodium borate, molybdenum oxide, expanded graphite, and tricresyl phosphate, etc.

[0003] Expanded graphite is increasingly being used as an effective flame retardant. Expanded graphite is an intercalated (sulfuric acid) graphite material that, when exposed to a heat source, can rapidly expand to 300 times its initial volume, forming a worm-like expanded layer. This expanded layer acts as a barrier to the transfer of heat and substances (oxygen, combustible gases) and reduces dripping. It is used in foams, coatings, and plastics to impart flame-retardant properties.

[0004] Many intumescent fire-retardant materials, due to their inherent expansibility, present challenges when used in colloidal materials. Firstly, the viscoelasticity of the colloidal material affects the expansion process of the intumescent fire-retardant. Secondly, the expansion of the intumescent fire-retardant can cause separation between the filler and the colloid, thus reducing the overall performance of the fire-retardant rubber. After separation, numerous cavities are formed within the colloid, which can easily lead to tearing of the colloid and reduce its stability during use. Summary of the Invention

[0005] The purpose of this invention is to provide a multi-layer composite fabric, so as to achieve the goal of providing a soft fabric with good flame retardant properties.

[0006] To achieve the above objectives, the present invention employs the following technical means:

[0007] A multi-layer composite fabric is made by sequentially bonding a fluororubber sheet, a flame-retardant fluorosilicone rubber sheet, a fabric layer, and a neoprene rubber sheet. The fluororubber sheet serves as the outer fabric, and the neoprene rubber sheet serves as the inner fabric. The fluororubber sheet and the flame-retardant fluorosilicone rubber sheet are hot-pressed together to form an outer layer, and the edges of the outer layer are hot-pressed and fused together with the edges of the neoprene rubber sheet.

[0008] The flame-retardant fluorosilicone rubber sheet is prepared by vulcanization under irradiation conditions.

[0009] Preferably, the flame-retardant fluorosilicone rubber sheet comprises, by weight, 100-200 parts of fluorosilicone rubber, 10-20 parts of additives, vermiculite powder and expandable graphite powder, wherein the total amount of vermiculite powder and expandable graphite powder added is 1%-5% of the mass of the fluorosilicone rubber, and the additives include asphalt and eucommia gum.

[0010] The fluorosilicone rubber, vermiculite, and expandable graphite powder are mixed under room temperature irradiation conditions to prepare a first precursor.

[0011] The first precursor, after being mixed, is mixed with the additive at room temperature to produce the second precursor;

[0012] The second precursor is vulcanized under heating and irradiation conditions.

[0013] Furthermore, the expandable graphite and the vermiculite powder are added in a ratio of 1 to 2:1.

[0014] Furthermore, the additives include 5-8 parts by weight of asphalt and 1-4 parts by weight of eucommia gum.

[0015] Furthermore, the first precursor is compounded at a dose of 5-30 kGy.

[0016] Furthermore, the second precursor is vulcanized at a dose of 20-60 kGy and at 50-70°C.

[0017] The present invention has the following beneficial effects during use:

[0018] It provides good protection against carbon monoxide, hydrochloric acid, hydrogen cyanide, 50% hydrogen peroxide, 10-30% nitric acid, potassium cyanide, sulfuric acid, nitric acid, hydrochloric acid, sodium hydroxide, acetone, aniline, carbon monoxide, 50% hydrogen peroxide, hydrogen sulfide, mercury, and 25% sulfuric acid.

[0019] Meanwhile, by irradiating and vulcanizing the rubber matrix, the fluorosilicone rubber filled with vermiculite and expanded graphite does not affect the softness of the fluorosilicone rubber during normal use. Furthermore, during the flame retardant process, even if the vermiculite and expandable graphite expand, they will not peel off from the fluorosilicone rubber body. This ensures the softness of the wearable material while effectively preventing the expanded material from peeling off from the matrix and affecting the flame retardant effect.

[0020] In addition, the present invention also provides a method for preparing fire protective clothing by irradiation, which solves the problem that existing fabrics are prone to separation between the matrix and the filler due to the expansion of the filling material after the use of expandable filler, and at the same time affects the softness of the matrix during normal use.

[0021] To solve the above problems, the present invention employs the following technical means:

[0022] A method for preparing fire-fighting protective clothing by irradiation includes irradiation mixing of filler and raw rubber to form a first mixed product, followed by room temperature mixing with additives; after room temperature mixing, vulcanization is carried out under irradiation conditions.

[0023] Furthermore, the filler includes vermiculite powder and expandable graphite powder, and the vermiculite powder and expandable graphite powder are mixed evenly and then added to the raw rubber.

[0024] Furthermore, the raw rubber is fluorosilicone rubber raw rubber.

[0025] Furthermore, the irradiation mixing is carried out at a dose of 5-30 kGy, and the vulcanization is carried out at a dose of 20-60 kGy and at a temperature of 50-70°C.

[0026] The present invention provides a preparation method in which a rubber matrix is ​​vulcanized with expandable graphite and vermiculite powder by irradiation vulcanization. By changing the irradiation, the bonding sites on the surface of the filler are changed, making the bonding between the filler and the matrix more stable. On the other hand, by using a quantitative dose of irradiation vulcanization, the rubber matrix can better adapt to the expansion of the expandable filler and provide good deformation cavity. Even if the raw rubber forms a certain network structure after vulcanization, it can still adapt well to the expansion of expandable graphite and vermiculite. Detailed Implementation

[0027] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0028] Therefore, the following detailed description of embodiments of the present invention is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0029] It should be noted that, unless otherwise specified, the embodiments and features described in this invention can be combined with each other.

[0030] Example 1

[0031] A multi-layer composite fabric is made by sequentially bonding a fluororubber sheet, a flame-retardant fluorosilicone rubber sheet, a fabric layer, and a neoprene rubber sheet. The fluororubber sheet serves as the outer fabric, and the neoprene rubber sheet serves as the inner fabric. The fluororubber sheet and the flame-retardant fluorosilicone rubber sheet are hot-pressed together to form an outer layer, and the edges of the outer layer are hot-pressed and fused together with the edges of the neoprene rubber sheet.

[0032] The flame-retardant fluorosilicone rubber sheet is prepared by vulcanization under irradiation conditions.

[0033] Specifically, the flame-retardant fluorosilicone rubber sheet comprises, by weight, 100 parts of fluorosilicone rubber, 10 parts of additives, vermiculite powder and expandable graphite powder. The total amount of vermiculite powder and expandable graphite powder added is 1% of the mass of the fluorosilicone rubber. The additives include asphalt and eucommia gum.

[0034] The fluorosilicone rubber, vermiculite, and expandable graphite powder are mixed under room temperature irradiation conditions to prepare a first precursor.

[0035] The first precursor, after being mixed, is mixed with the additive at room temperature to produce the second precursor;

[0036] The second precursor is vulcanized under heating and irradiation conditions.

[0037] The expandable graphite and the vermiculite powder are added in a 1:1 ratio.

[0038] The additives include 5 parts by weight of asphalt and 1 part by weight of eucommia gum.

[0039] The first precursor was compounded at a dose of 5 kGy.

[0040] The second precursor was vulcanized at a dose of 20 kGy and at 50°C.

[0041] Irradiation is carried out in the following manner: irradiation mixing of filler and raw rubber to form the first mixed product, followed by room temperature mixing with additives; after room temperature mixing, vulcanization is carried out under irradiation conditions.

[0042] The filler includes vermiculite powder and expandable graphite powder, which are mixed evenly and then added to the raw rubber.

[0043] The raw rubber is fluorosilicone rubber raw rubber.

[0044] The irradiation mixing was carried out at a dose of 5 kGy, and the vulcanization was carried out at a dose of 20 kGy and at 50°C.

[0045] Example 2

[0046] A multi-layer composite fabric is made by sequentially bonding a fluororubber sheet, a flame-retardant fluorosilicone rubber sheet, a fabric layer, and a neoprene rubber sheet. The fluororubber sheet serves as the outer fabric, and the neoprene rubber sheet serves as the inner fabric. The fluororubber sheet and the flame-retardant fluorosilicone rubber sheet are hot-pressed together to form an outer layer, and the edges of the outer layer are hot-pressed and fused together with the edges of the neoprene rubber sheet.

[0047] The flame-retardant fluorosilicone rubber sheet is prepared by vulcanization under irradiation conditions.

[0048] Specifically, the flame-retardant fluorosilicone rubber sheet comprises, by weight, 200 parts of fluorosilicone rubber, 20 parts of additives, vermiculite powder and expandable graphite powder. The total amount of vermiculite powder and expandable graphite powder added is 5% of the mass of the fluorosilicone rubber. The additives include asphalt and eucommia gum.

[0049] The fluorosilicone rubber, vermiculite, and expandable graphite powder are mixed under room temperature irradiation conditions to prepare a first precursor.

[0050] The first precursor, after being mixed, is mixed with the additive at room temperature to produce the second precursor;

[0051] The second precursor is vulcanized under heating and irradiation conditions.

[0052] The expandable graphite and the vermiculite powder are added in a ratio of 2:1.

[0053] The additives include 8 parts by weight of asphalt and 4 parts by weight of eucommia gum.

[0054] The first precursor was compounded at a dose of 30 kGy.

[0055] The second precursor was vulcanized at a dose of 60 kGy and at 70°C.

[0056] Irradiation is carried out in the following manner: irradiation mixing of filler and raw rubber to form the first mixed product, followed by room temperature mixing with additives; after room temperature mixing, vulcanization is carried out under irradiation conditions.

[0057] The filler includes vermiculite powder and expandable graphite powder, which are mixed evenly and then added to the raw rubber.

[0058] The raw rubber is fluorosilicone rubber raw rubber.

[0059] The irradiation mixing was carried out at a dose of 30 kGy, and the vulcanization was carried out at a dose of 60 kGy and a temperature of 70°C.

[0060] Example 3

[0061] A multi-layer composite fabric is made by sequentially bonding a fluororubber sheet, a flame-retardant fluorosilicone rubber sheet, a fabric layer, and a neoprene rubber sheet. The fluororubber sheet serves as the outer fabric, and the neoprene rubber sheet serves as the inner fabric. The fluororubber sheet and the flame-retardant fluorosilicone rubber sheet are hot-pressed together to form an outer layer, and the edges of the outer layer are hot-pressed and fused together with the edges of the neoprene rubber sheet.

[0062] The flame-retardant fluorosilicone rubber sheet is prepared by vulcanization under irradiation conditions.

[0063] Specifically, the flame-retardant fluorosilicone rubber sheet comprises, by weight, 150 parts of fluorosilicone rubber, 15 parts of additives, vermiculite powder and expandable graphite powder. The total amount of vermiculite powder and expandable graphite powder added is 3% of the mass of the fluorosilicone rubber. The additives include asphalt and eucommia gum.

[0064] The fluorosilicone rubber, vermiculite, and expandable graphite powder are mixed under room temperature irradiation conditions to prepare a first precursor.

[0065] The first precursor, after being mixed, is mixed with the additive at room temperature to produce the second precursor;

[0066] The second precursor is vulcanized under heating and irradiation conditions.

[0067] The expandable graphite and the vermiculite powder are added in a ratio of 1.5:1.

[0068] The additives include 6 parts by weight of asphalt and 3 parts by weight of eucommia gum.

[0069] The first precursor was compounded at a dose of 20 kGy.

[0070] The second precursor was vulcanized at a dose of 40 kGy and at 60 °C.

[0071] Irradiation is carried out in the following manner: irradiation mixing of filler and raw rubber to form the first mixed product, followed by room temperature mixing with additives; after room temperature mixing, vulcanization is carried out under irradiation conditions.

[0072] The filler includes vermiculite powder and expandable graphite powder, which are mixed evenly and then added to the raw rubber.

[0073] The raw rubber is fluorosilicone rubber raw rubber.

[0074] The irradiation mixing was carried out at a dose of 20 kGy, and the vulcanization was carried out at a dose of 40 kGy and a temperature of 60°C.

[0075] Comparative Example 1

[0076] The sulfidation process in Example 3 was selected from sulfidation under natural conditions.

[0077] The fabrics prepared in Examples 1, 2, 3, and Comparative Example 1 were subjected to mechanical property tests:

[0078]

[0079] In addition, flame retardant performance tests were conducted on Examples 1, 2, 3, and Comparative Example 1. After testing, the flame retardant performance of Examples 1 to 3 was significantly better than that of Comparative Example 1. Furthermore, during the carbonization process, Comparative Example 1 experienced severe edge curling and a large amount of particle shedding. In contrast, Example 3, as the optimal example, showed virtually no burning particles shedding during the carbonization process, and almost no edge curling occurred at the carbonized location.

[0080] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. 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 multi-layer composite fabric, characterized in that: It is made by sequentially bonding a fluororubber sheet, a flame-retardant fluorosilicone rubber sheet, a fabric layer, and a neoprene rubber sheet. The fluororubber sheet serves as the outer fabric, and the neoprene rubber sheet serves as the inner fabric. The fluororubber sheet and the flame-retardant fluorosilicone rubber sheet are hot-pressed together to form an outer layer. The edge of the outer layer is hot-pressed and fused to the edge of the neoprene rubber sheet. The flame-retardant fluorosilicone rubber sheet is prepared by vulcanization under irradiation conditions; The flame-retardant fluorosilicone rubber sheet comprises, by weight, 100-200 parts of fluorosilicone rubber, 10-20 parts of additives, vermiculite powder and expandable graphite powder. The total amount of vermiculite powder and expandable graphite powder added is 1%-5% of the mass of the fluorosilicone rubber. The additives include asphalt and eucommia gum. The fluorosilicone rubber is mixed with the vermiculite powder and the expandable graphite powder under room temperature irradiation conditions to prepare a first precursor; The first precursor, after being mixed, is mixed with the additive at room temperature to produce the second precursor; The second precursor is vulcanized under heating and irradiation conditions.

2. The multilayer composite fabric according to claim 1, characterized in that: The expandable graphite powder and the vermiculite powder are added in a ratio of 1 to 2:

1.

3. The multilayer composite fabric according to claim 1, characterized in that: The additives include 5-8 parts by weight of asphalt and 1-4 parts by weight of eucommia gum.

4. The multilayer composite fabric according to claim 1, characterized in that: In the process of preparing the first precursor, the mixture is compounded at a dose of 5 to 30 kGy.

5. The multilayer composite fabric according to claim 1, characterized in that: The second precursor is vulcanized at a dose of 20-60 kGy and at 50-70°C.

6. A method for preparing a multilayer composite fabric as described in any one of claims 1 to 5, characterized in that: The process includes irradiation mixing of fillers and raw fluorosilicone rubber to form a first precursor, followed by room temperature mixing with additives; after room temperature mixing, vulcanization is carried out under irradiation conditions. The filler includes vermiculite powder and expandable graphite powder, which are mixed evenly and then added to the fluorosilicone rubber raw material.

7. The preparation method according to claim 6, characterized in that: The irradiation mixing is carried out at a dose of 5-30 kGy, and the vulcanization is carried out at a dose of 20-60 kGy and at a temperature of 50-70°C.

Citation Information

Patent Citations

  • Composite fluororubber adhesive plaster and preparation method thereof

    CN102501481A

  • Method for improving performances of rubber roller apron

    CN110204747A

  • Flame-retardant fluorinated silicone rubber foam composite material and preparation process thereof

    CN115230188A