Preparation method of composite flame-retardant waterproof material

Abstract

The invention discloses a preparation method of a composite flame-retardant waterproof material, relates to the technical field of flame-retardant waterproof materials, and aims to solve the technical problem that a traditional single material often difficultly meets flame-retardant and waterproof requirements at the same time, and the preparation method comprises the following steps: S1, raw material selection; bisphenol A type epoxy resin with the purity not lower than 99% is selected as a base material, and the epoxy value of the bisphenol A type epoxy resin is controlled between 0.45 mol / 100g and 0.6 mol / 100g, so that good crosslinking property and mechanical property are ensured; s2, performing pretreatment; the preparation method comprises the following steps: placing epoxy resin in a vacuum drying oven, and drying for 4-8 hours at the temperature of 80-100 DEG C to remove moisture and volatile matters so as to avoid adverse effects on subsequent processes; s3, constructing and optimizing a flame retardant system; the preparation method comprises the following steps: accurately weighing a phosphorus-based flame retardant and a halogen-based flame retardant according to the mass ratio of the PBPP to the decabromodiphenyl ethane of (1: 1)-(3: 1), uniformly mixing, and ensuring that the addition amount of the flame retardants is 5-15% of the total mass; the flame-retardant waterproof fabric has the advantage of simultaneously realizing flame-retardant and waterproof effects.

Description

Technical Field

[0001] The invention relates to the technical field of flame retardant and waterproof materials, and more specifically to a method for preparing a composite flame retardant and waterproof material. Background Art

[0002] Flame retardant and waterproof materials are materials that have the characteristics of inhibiting or delaying combustion. They can prevent the occurrence or spread of fire to a certain extent, and at the same time have good waterproof properties. With the rapid development of science and technology and industry, the requirements for material performance are increasing, especially in the field of strict requirements on safety, durability and environmental friendliness. Traditional single materials are often difficult to meet the flame retardant and waterproof requirements at the same time. In view of this, we propose a preparation method of a composite flame retardant and waterproof material. Summary of the invention

[0003] The purpose of the present invention is to provide a method for preparing a composite flame retardant and waterproof material to solve the technical problem that traditional single materials are often difficult to simultaneously meet the flame retardant and waterproof requirements.

[0004] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for preparing a composite flame retardant and waterproof material, comprising the following steps:

[0005] S1. Raw material selection;

[0006] Bisphenol A epoxy resin with a purity of not less than 99% is selected as the base material, and its epoxy value is controlled between 0.45 and 0.6 mol / 100g to ensure good cross-linking and mechanical properties;

[0007] S2, pre-processing;

[0008] Place the epoxy resin in a vacuum drying oven and dry it at 80°C to 100°C for 4-8 hours to remove moisture and volatiles to avoid adverse effects on subsequent processes;

[0009] S3, flame retardant system construction and optimization;

[0010] According to the mass ratio of polyphenoxy biphenyl phosphate ester PBPP to decabromodiphenyl ethane of 1:1-3:1, accurately weigh the phosphorus flame retardant and the halogen flame retardant, mix them evenly, and ensure that the addition amount of the flame retardant is between 5% and 15% of the total mass;

[0011] S4, adding waterproofing agent and additives;

[0012] Select a silicone waterproofing agent that is compatible with epoxy resin and control the content between 1% and 3% of the total mass to ensure that the material has excellent waterproof performance;

[0013] Adding a carboxyl-terminated nitrile rubber toughening agent, a polysiloxane leveling agent, and a hindered phenol antioxidant to the mixed system in sequence and stirring them evenly, wherein the amount of the carboxyl-terminated nitrile rubber added is 2%-5% of the total mass, the amount of the polysiloxane leveling agent added is 0.1%-0.5% of the total mass, and the amount of the hindered phenol antioxidant added is 0.1%-0.3% of the total mass;

[0014] S5, efficient mixing and dispersion;

[0015] Use a high-speed disperser to evenly disperse the flame retardant, waterproofing agent and other additives into the epoxy resin at a speed of 2000-4000rpm;

[0016] Introducing ultrasonic dispersion equipment at a frequency of 20kHz to 40kHz for 30 minutes to 1 hour to further refine the particles and improve the uniformity and stability of the mixture;

[0017] S6, vacuum degassing and precision curing;

[0018] Transfer the evenly mixed material to a vacuum degassing machine and degas for 30 min to 1 h at a vacuum degree of -0.1 MPa to -0.08 MPa to completely remove bubbles;

[0019] Precision curing process: first pre-curing at room temperature for 2-4 hours, then post-curing at a low temperature of 60℃-80℃ for 4-8 hours, and finally final curing at a high temperature of 120℃-150℃ for 2-4 hours. Through the step-by-step curing process, the epoxy resin is fully cross-linked to form a dense network structure.

[0020] S7, finished product inspection and quality control;

[0021] The cured composite materials are subjected to rigorous performance tests, including UL-94 flame retardant rating test, hydrostatic pressure test, tensile strength test, flexural strength test and weather resistance test;

[0022] Grading and screening are carried out based on the test results to ensure that all products meet the preset performance indicators and quality standards.

[0023] Preferably, in S2, the pretreatment of the epoxy resin further includes preliminary screening before vacuum drying to remove impurities and unqualified particles, thereby further improving the purity of the epoxy resin and the stability of subsequent processes.

[0024] Preferably, in S3, the flame retardant system also includes one of hydroxide or magnesium hydroxide, and the addition amount thereof accounts for 1%-10% of the total mass, so as to further enhance the flame retardant properties of the material and reduce the toxicity of smoke during combustion.

[0025] Preferably, in S4, the organosilicon waterproofing agent is specially modified to improve its dispersibility and compatibility in the epoxy resin, thereby further improving the waterproofing effect.

[0026] Preferably, in S5, the ultrasonic dispersion treatment further includes controlling the temperature of the dispersion liquid to maintain it between 20° C. and 40° C. to optimize the propagation effect of the ultrasonic wave and the particle refinement efficiency.

[0027] Preferably, an intelligent control system and online monitoring technology are introduced to monitor and adjust key process parameters such as mixing, dispersion, and curing in real time to ensure the stability and consistency of product quality.

[0028] Preferably, the intelligent control system also includes a data analysis module for collecting and analyzing real-time data in the mixing, dispersion, solidification and other processes, predicting and preventing potential quality problems, and improving the intelligence level of the production process.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] 1. The present invention designs vacuum degassing and precision curing steps, and degasses for 30 min-1 h at a vacuum degree of -0.1 MPa to -0.08 MPa, which is conducive to completely removing bubbles, thereby ensuring the density of the mixed material and eliminating the influence of residual bubbles on the flame retardant and waterproof properties of the material, thereby designing a material that meets both flame retardant and waterproof effects, solving the problem that traditional single materials are often difficult to meet the flame retardant and waterproof requirements at the same time.

[0031] 2. The present invention also designs precise curing process steps to achieve step-by-step curing of the material at room temperature, 60°C-80°C and 120°C-150°C, respectively, which is beneficial to improving the curing effect of the material, allowing the epoxy resin to be fully cross-linked to form a dense network structure, thereby improving the flame retardant and waterproof properties of the material. DETAILED DESCRIPTION

[0032] In order to facilitate those skilled in the art to understand the technical solution of the present invention, the technical solution of the present invention is further explained in conjunction with the specification.

[0033] A method for preparing a composite flame retardant and waterproof material comprises the following steps:

[0034] S1. Raw material selection;

[0035] Bisphenol A epoxy resin with a purity of not less than 99% is selected as the base material, and its epoxy value is controlled between 0.45 and 0.6 mol / 100g to ensure good cross-linking and mechanical properties;

[0036] S2, pre-processing;

[0037] Place the epoxy resin in a vacuum drying oven and dry it at 80°C to 100°C for 4-8 hours to remove moisture and volatiles to avoid adverse effects on subsequent processes;

[0038] S3, flame retardant system construction and optimization;

[0039] According to the mass ratio of polyphenoxy biphenyl phosphate ester PBPP to decabromodiphenyl ethane of 1:1-3:1, accurately weigh the phosphorus flame retardant and the halogen flame retardant, mix them evenly, and ensure that the addition amount of the flame retardant is between 5% and 15% of the total mass;

[0040] S4, adding waterproofing agent and additives;

[0041] Select a silicone waterproofing agent that is compatible with epoxy resin and control the content between 1% and 3% of the total mass to ensure that the material has excellent waterproof performance;

[0042] Adding a carboxyl-terminated nitrile rubber toughening agent, a polysiloxane leveling agent, and a hindered phenol antioxidant to the mixed system in sequence and stirring them evenly, wherein the amount of the carboxyl-terminated nitrile rubber added is 2%-5% of the total mass, the amount of the polysiloxane leveling agent added is 0.1%-0.5% of the total mass, and the amount of the hindered phenol antioxidant added is 0.1%-0.3% of the total mass;

[0043] S5, efficient mixing and dispersion;

[0044] Use a high-speed disperser to evenly disperse the flame retardant, waterproofing agent and other additives into the epoxy resin at a speed of 2000-4000rpm;

[0045] Introducing ultrasonic dispersion equipment at a frequency of 20kHz to 40kHz for 30 minutes to 1 hour to further refine the particles and improve the uniformity and stability of the mixture;

[0046] S6, vacuum degassing and precision curing;

[0047] Transfer the evenly mixed material to a vacuum degassing machine and degas for 30 min to 1 h at a vacuum degree of -0.1 MPa to -0.08 MPa to completely remove bubbles;

[0048] Precision curing process: first pre-curing at room temperature for 2-4 hours, then post-curing at a low temperature of 60℃-80℃ for 4-8 hours, and finally final curing at a high temperature of 120℃-150℃ for 2-4 hours. Through the step-by-step curing process, the epoxy resin is fully cross-linked to form a dense network structure.

[0049] S7, finished product inspection and quality control;

[0050] The cured composite materials are subjected to rigorous performance tests, including UL-94 flame retardant rating test, hydrostatic pressure test, tensile strength test, flexural strength test and weather resistance test;

[0051] Grading and screening are carried out based on the test results to ensure that all products meet the preset performance indicators and quality standards.

[0052] In S2, the pretreatment of epoxy resin also includes preliminary screening before vacuum drying to remove impurities and unqualified particles, so as to further improve the purity of epoxy resin and the stability of subsequent processes. In S3, the components of the flame retardant system also include one of hydroxide or magnesium hydroxide, and the addition amount accounts for 1%-10% of the total mass to further enhance the flame retardant properties of the material and reduce the toxicity of smoke during combustion. In S4, the silicone waterproofing agent is specially modified to improve its dispersibility and compatibility in epoxy resin, so as to further enhance the waterproof effect. In S5, the ultrasonic dispersion treatment also includes temperature control of the dispersion liquid, which is maintained between 20℃ and 40℃ to optimize the propagation effect of ultrasonic waves and the efficiency of particle refinement. Intelligent control systems and online monitoring technologies are introduced to monitor and adjust key process parameters such as mixing, dispersion, and curing in real time to ensure the stability and consistency of product quality. The intelligent control system also includes a data analysis module for collecting and analyzing real-time data in the mixing, dispersion, and curing processes, predicting and preventing potential quality problems, and improving the intelligence level of the production process.

[0053] The embodiments of the present invention disclose preferred embodiments, but are not limited thereto. A person skilled in the art can easily understand the spirit of the present invention based on the above embodiments and make different extensions and changes. However, as long as they do not deviate from the spirit of the present invention, they are all within the protection scope of the present invention.

Claims

1. A method for preparing a composite flame retardant and waterproof material, characterized in that: The following steps are involved: S1. Raw material selection; Bisphenol A epoxy resin with a purity of not less than 99% is selected as the base material, and its epoxy value is controlled between 0.45 and 0.6 mol / 100g to ensure good cross-linking and mechanical properties; S2, pre-processing; Place the epoxy resin in a vacuum drying oven and dry it at 80°C to 100°C for 4-8 hours to remove moisture and volatiles to avoid adverse effects on subsequent processes; S3, flame retardant system construction and optimization; According to the mass ratio of polyphenoxy biphenyl phosphate ester PBPP to decabromodiphenyl ethane of 1:1-3:1, accurately weigh the phosphorus flame retardant and the halogen flame retardant, mix them evenly, and ensure that the addition amount of the flame retardant is between 5% and 15% of the total mass; S4, adding waterproofing agent and additives; Select a silicone waterproofing agent that is compatible with epoxy resin and control the content between 1% and 3% of the total mass to ensure that the material has excellent waterproof performance; Adding a carboxyl-terminated nitrile rubber toughening agent, a polysiloxane leveling agent, and a hindered phenol antioxidant to the mixed system in sequence and stirring them evenly, wherein the amount of the carboxyl-terminated nitrile rubber added is 2%-5% of the total mass, the amount of the polysiloxane leveling agent added is 0.1%-0.5% of the total mass, and the amount of the hindered phenol antioxidant added is 0.1%-0.3% of the total mass; S5, efficient mixing and dispersion; Use a high-speed disperser to evenly disperse the flame retardant, waterproofing agent and other additives into the epoxy resin at a speed of 2000-4000rpm; Introducing ultrasonic dispersion equipment at a frequency of 20kHz to 40kHz for 30 minutes to 1 hour to further refine the particles and improve the uniformity and stability of the mixture; S6, vacuum degassing and precision curing; Transfer the evenly mixed material to a vacuum degassing machine and degas for 30 min to 1 h at a vacuum degree of -0.1 MPa to -0.08 MPa to completely remove bubbles; Precision curing process: first pre-curing at room temperature for 2-4 hours, then post-curing at a low temperature of 60℃-80℃ for 4-8 hours, and finally final curing at a high temperature of 120℃-150℃ for 2-4 hours. Through the step-by-step curing process, the epoxy resin is fully cross-linked to form a dense network structure. S7, finished product inspection and quality control; The cured composite materials are subjected to rigorous performance tests, including UL-94 flame retardant rating test, hydrostatic pressure test, tensile strength test, flexural strength test and weather resistance test; Grading and screening are carried out based on the test results to ensure that all products meet the preset performance indicators and quality standards.

2. The method for preparing a composite flame retardant and waterproof material according to claim 1, characterized in that: In S2, the pretreatment of the epoxy resin also includes preliminary screening before vacuum drying to remove impurities and unqualified particles, thereby further improving the purity of the epoxy resin and the stability of subsequent processes.

3. The method for preparing a composite flame retardant and waterproof material according to claim 1, characterized in that: In S3, the flame retardant system also includes one of hydroxide or magnesium hydroxide, and the addition amount thereof accounts for 1%-10% of the total mass, so as to further enhance the flame retardant properties of the material and reduce the toxicity of smoke during combustion.

4. The method for preparing a composite flame retardant and waterproof material according to claim 1, characterized in that: In S4, the organosilicon waterproofing agent is specially modified to improve its dispersibility and compatibility in the epoxy resin, thereby further improving the waterproofing effect.

5. The method for preparing a composite flame retardant and waterproof material according to claim 1, characterized in that: In S5, the ultrasonic dispersion treatment further includes controlling the temperature of the dispersion liquid to maintain it between 20° C. and 40° C. to optimize the propagation effect of the ultrasonic wave and the particle refinement efficiency.

6. The method for preparing a composite flame retardant and waterproof material according to claim 1, characterized in that: Intelligent control systems and online monitoring technologies are introduced to monitor and adjust key process parameters such as mixing, dispersion, and curing in real time to ensure the stability and consistency of product quality.

7. The method for preparing a composite flame retardant and waterproof material according to claim 6, characterized in that: The intelligent control system also includes a data analysis module, which is used to collect and analyze real-time data during the mixing, dispersion, and solidification processes, predict and prevent potential quality problems, and improve the intelligence level of the production process.