High-performance floating bag based on multi-technology cooperation and preparation method thereof

By modifying the fiber fabric with silane coupling agent and using a two-stage mixing process with m-methyl silica composite material, combined with low-temperature segmented vulcanization, the problems of interfacial bonding strength and sealing performance in the preparation of floats were solved, realizing the preparation of high-performance floats and improving the reliability and lifespan of the products.

CN121870979APending Publication Date: 2026-04-17YUNNAN ADVANCED ELASTOMER IND INNOVATION RES INST CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
YUNNAN ADVANCED ELASTOMER IND INNOVATION RES INST CO LTD
Filing Date
2026-02-09
Publication Date
2026-04-17

AI Technical Summary

Technical Problem

Existing float preparation technologies suffer from problems such as fiber thermal oxidative degradation, insufficient interfacial bonding strength, microscopic defects, and poor sealing, making it difficult to meet the requirements for high reliability and long service life.

Method used

By using silane coupling agent to modify fiber fabric, combined with m-methyl silica composite rubber and optimized two-stage mixing process, and through low-temperature segmented vulcanization process, a chemical bonding layer and defect-free bonding interface are constructed to achieve high bonding strength and excellent sealing performance of the float.

Benefits of technology

It significantly improves the bonding strength and sealing reliability of the float, reduces the performance degradation rate after long-term fatigue cycles and media immersion, and provides a float product with high reliability and long service life.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of preparation of floating bag materials, and discloses a high-performance floating bag based on multi-technology synergy and a preparation method thereof.The preparation method comprises the following steps that S1, a fiber fabric is subjected to alkaline cleaning, then washed with water and dried, modified with a silane coupling agent and dried, and a pretreated fabric is obtained; s2, weighing the rubber material according to the formula, performing two-stage mixing by an internal mixer, discharging sheets, and standing and curing for at least 24 hours to obtain rubber sheets; the preparation method comprises the following steps: dissolving sizing materials with the same formula in an organic solvent to prepare 15-25wt% of adhesive cement, spraying the adhesive cement on the surface of a rubber sheet, and airing for 10-15 minutes to obtain a pretreated rubber sheet; s3, laminating the pretreated film and the pretreated fabric in a clean environment, and rolling to remove bubbles to obtain a preset floating bag material; and S4, the preset floating bag material is put into the mold, differential pressure is applied to the long edge, the short edge and the air inlet and outlet through the segmented mold, timing vulcanization is started, demolding is conducted after vulcanization is completed, and the floating bag is obtained.
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Description

Technical Field

[0001] This invention relates to the field of float material preparation technology, specifically to a high-performance float based on multi-technology synergy and its preparation method. Background Technology

[0002] A float is an inflatable buoyancy component made of high-strength rubber-coated fabric. It can be fitted to unmanned underwater vehicles, experimental underwater devices, and underwater salvage equipment to provide buoyancy assistance to negatively buoyant underwater vehicles, facilitating subsequent salvage and recovery operations. A float typically consists of a high-pressure gas cylinder, a solenoid valve, and a differential pressure sensor to form a complete buoyancy system. In normal operation, the float is folded and stored in a recess within the underwater device's casing, with an external deflector maintaining the device's streamlined shape. When the underwater device completes its planned navigation mission or encounters an emergency, the control module issues an inflation command and triggers the solenoid valve. High-pressure gas from the cylinder enters the float through a pipeline, causing it to expand rapidly. Simultaneously, the deflector opens. The differential pressure sensor and safety valve on the float precisely control the internal pressure to prevent over-inflation and component damage. The inflated float provides sufficient positive buoyancy for the underwater device, allowing it to rise smoothly to the surface.

[0003] Current float fabrication methods largely employ traditional high-temperature vulcanization bonding technology, which has significant technical drawbacks that severely restrict product reliability and lifespan. Firstly, the high-temperature vulcanization environment of traditional processes easily leads to thermal oxidative degradation of the fibers in nylon or aramid fabric substrates, significantly weakening the overall structural strength and tear resistance of the float. Secondly, volatile components within the rubber compound rapidly precipitate during vulcanization. Due to lax process control, imperceptible defects such as internal bubbles and delamination easily form at the rubber-fabric interface. These microscopic defects become sources of media penetration and stress concentration, severely compromising the float's sealing integrity. Furthermore, traditional vulcanization systems generally have poor formulation compatibility. The interfacial bonding between rubber and high-strength fabric relies primarily on physical anchoring and weak van der Waals forces, resulting in weak chemical bonds and insufficient bond strength. This makes it difficult to meet the stringent operating conditions faced by floaters in actual use, including repeated high-pressure inflation and deflation, long-term seawater immersion corrosion, and complex fluid pressure variations. Furthermore, a single surface treatment technique or simple mechanical polishing cannot completely remove the weak boundary layer on the fiber surface and introduce highly active reaction sites, making it difficult to form a stable, chemically bonded interfacial transition layer between the substrate and the adhesive. This fundamental limitation further restricts the service life and long-term reliability of the float.

[0004] Therefore, the industry urgently needs an innovative fabrication solution that can systematically address the coordination and unification of interface bonding, defect control, and low-temperature molding. Based on this, this application provides a high-performance float based on multi-technology synergy and its fabrication method. Summary of the Invention

[0005] Technical problems to be solved To address the shortcomings of existing technologies, this invention provides a high-performance floatation bag based on multi-technology synergy and its preparation method.

[0006] Technical solution To achieve the above objectives, the present invention provides the following technical solution: A method for preparing a high-performance float based on multi-technology synergy specifically includes the following steps: S1. After alkaline cleaning of the fiber fabric, it is washed with water, dried, modified with a silane coupling agent, and then dried to obtain the pretreated fabric. S2. Weigh the rubber compound according to the formula, mix it in two stages using an internal mixer, and then sheet it out. Let it stand and mature for at least 24 hours to obtain the rubber sheet. Dissolve the same rubber compound in an organic solvent to prepare a 15-25wt% rubber paste, spray it on the surface of the rubber sheet, and let it air dry in a ventilated and dust-free environment for 10-15 minutes to obtain the pretreated rubber sheet. The organic solvent is at least one of toluene, xylene, No. 120 gasoline, or a special rubber solvent.

[0007] S3. Precisely bond the pre-treated film and the pre-treated fabric in a clean environment, roll them to remove air bubbles, and obtain the pre-shaped float material. S4. Place the pre-shaped float material into the mold, apply differentiated pressure to the long side, short side, and air inlet / outlet through the segmented mold, and start timing vulcanization. After vulcanization is completed, allow it to cool naturally to below 60°C before demolding to obtain the float.

[0008] Furthermore, the pretreated fabric is specifically prepared by the following steps: The fiber fabric is immersed in an alkaline washing solution at 50-60℃ and ultrasonically treated for 5-10 minutes; then rinsed until neutral and dried; the dried fiber fabric is sprayed with a silane coupling agent solution, and then dried and cured to obtain the pretreated fabric.

[0009] Furthermore, the pretreated fabric is specifically prepared by the following steps: The fiber fabric is immersed in an alkaline detergent solution at a liquor ratio of 1g:20mL at 50-60℃ and ultrasonically treated for 5-10 minutes. Then it is rinsed with deionized water until neutral and dried with hot air at 60-80℃. The dried fiber fabric is then sprayed with a silane coupling agent solution and dried and cured at 110-120℃ for 3-5 minutes to obtain the pretreated fabric.

[0010] In the above steps, surface impurities such as textile oils and release agents on the fiber fabric are removed by alkaline washing solution and ultrasonic treatment, thereby increasing the surface energy. Subsequently, a silane coupling agent solution is used for modification. The silane coupling agent can form a chemically bonded layer on the fiber surface, significantly enhancing the interfacial bonding force with the subsequent rubber layer.

[0011] Furthermore, the alkaline washing solution is a 3-5 wt% sodium hydroxide solution.

[0012] Furthermore, the silane coupling agent solution is an ethanol solution of γ-aminopropyltriethoxysilane (hereinafter referred to as KH-550), and the content of KH-550 is 1-2 wt%.

[0013] Furthermore, the specific parameters for the spraying are: spray gun air pressure of 0.3-0.5 MPa, spraying distance of 15-25 cm, and gun travel speed of 0.3-0.6 m / s; the target dry film coating amount is 0.5-1.5 g / m³. 2 .

[0014] Furthermore, the ultrasonic treatment involves an ultrasonic power of 200-300W and an ultrasonic frequency of 25-40kHz.

[0015] Further, in step S2, the adhesive material specifically comprises the following parts by weight of raw materials: 100 parts natural rubber, 10-50 parts chloroprene rubber, 1-10 parts resorcinol resin, 1-10 parts formaldehyde donor, 25-35 parts silica, 5-6 parts activator, 1-1.5 parts stearic acid, 2-3 parts accelerator, 2-3 parts anti-aging agent, and 3-5 parts tackifying resin.

[0016] Further, in step S2, the adhesive material specifically comprises the following parts by weight of raw materials: 100 parts natural rubber, 20-30 parts chloroprene rubber, 4-6 parts resorcinol resin, 2-3 parts formaldehyde donor, 25-35 parts silica, 5-6 parts activator, 1-1.5 parts stearic acid, 2-3 parts accelerator, 2-3 parts anti-aging agent, and 3-5 parts tackifying resin.

[0017] Furthermore, the formaldehyde donor is at least one of hexamethylenetetramine, HMT-80, adhesive A, and adhesive RA / RH.

[0018] Furthermore, the activator is at least one of zinc oxide, zinc stearate, and nano zinc oxide.

[0019] More preferably, the activator is zinc oxide.

[0020] Furthermore, the accelerator is obtained by mixing accelerator M (2-mercaptobenzothiazole) and accelerator DM (dibenzothiazole disulfide) in a mass ratio of (2-3):1.

[0021] Furthermore, the anti-aging agent is obtained by mixing RD (2,2,4-trimethyl-1,2-dihydroquinoline polymer) and 4010NA (N-isopropyl-N'-phenyl-p-phenylenediamine) in a mass ratio of (2-3):1.

[0022] Furthermore, the tackifying resin is at least one of terpene resin, C5 petroleum resin, C9 petroleum resin, and modified alkylphenol resin.

[0023] Furthermore, the two-stage mixed training specifically includes the following steps: A1. Put natural rubber and chloroprene rubber into a mixer and masticate for 30-60 seconds. Then add 2 / 3 of the formula amount of resorcinol resin, activator, stearic acid, anti-aging agent and the full amount of formula amount of fumed silica. Sweep up the powder to ensure that all of it falls into the mixing chamber. Set the top pressure to 0.6-0.8MPa and mix at a rate of 60-80rpm until the system temperature rises to 145-155℃. When the rubber is discharged, cool and let it stand for 4-24 hours to obtain a first-stage rubber. A2. Add a section of adhesive to the internal mixer and control the mixing temperature within the range of 90-100℃. Then add the remaining 1 / 3 of the formula amount of resorcinol resin, activator, stearic acid, and anti-aging agent, and mix at a rate of 40-60 rpm for 2-3 minutes. Next, add the formaldehyde donor, accelerator, and tackifying resin according to the formula amount. Set the top pressure to 0.3-0.5 MPa and continue mixing. Control the discharge temperature to ≤110℃. Discharge the adhesive immediately after 30-60 seconds. After discharge, beat the adhesive in a triangular shape 5-8 times under the condition of roller temperature <50℃ for further homogenization and then produce sheets with a sheet thickness of 0.5-1.0 mm.

[0024] In the above technical solution, the order of adding materials in the mixing process is optimized to prevent the formaldehyde donor and resorcinol resin from undergoing premature resinification reaction at 90-100℃, which would lead to a decrease in the performance of the adhesive and ensure that the accelerator is evenly dispersed and does not react prematurely.

[0025] Among them, "triangular wrapping" refers to scraping the rubber compound off the rollers of the open mill and putting it back in to form a triangular cross section. In this technical solution, this is repeated 5-8 times to enhance the shear force and mixing effect.

[0026] Furthermore, in step S3, the rolling process specifically employs a three-roll calender to roll the rollers from the center to the edge at least three times. The speed ratio of the upper, middle, and lower rollers is 1:1.1-1.2:1.3-1.4. The temperature of the upper roller is set to 40-50℃, the temperature of the middle roller is set to 45-55℃, and the temperature of the lower roller is set to 50-60℃. The ambient temperature is controlled at 20-28℃, and the humidity is <60%.

[0027] Furthermore, the vulcanization is carried out using compression molding vulcanization or airbag pressurized vulcanization, specifically as follows: first, apply a pressure of 0.8 MPa to the entire material and preheat for 10 minutes to allow the rubber compound to flow and fill. Then, vulcanize the material according to the following parameters: long side vulcanization pressure 1.3-1.4 MPa, vulcanization time 110-150 minutes, vulcanization temperature 85-95℃; short side vulcanization pressure 1.0-1.1 MPa, vulcanization time 100-130 minutes, vulcanization temperature 85-95℃; air inlet and air outlet vulcanization pressure 1.6-1.7 MPa, vulcanization time 120-160 minutes, vulcanization temperature 85-95℃.

[0028] A high-performance float based on multi-technology collaboration.

[0029] Beneficial technical effects This invention utilizes a silane coupling agent to chemically modify the surface of fiber fabrics, constructing a robust chemical bond layer on the fiber surface and fundamentally improving the interfacial affinity and reactivity between the substrate and the adhesive. The use of a m-methyl silica composite adhesive system and an optimized two-stage mixing process ensures high crosslinking density and excellent media stability at low temperatures, while avoiding damage to the fibers at high temperatures. Activation treatment of the adhesive film surface using the adhesive paste, combined with the precise rolling operation of a three-roll calender, achieves perfect bonding between the rubber and fabric interface and complete elimination of micro-bubbles, constructing a defect-free adhesive interface.

[0030] The core innovation lies in implementing a segmented, differentiated low-temperature vulcanization process tailored to the structure and stress characteristics of different parts of the float. This allows key areas such as the long side, short side, and air inlet / outlet to receive appropriate curing pressure and time, thereby simultaneously achieving high bonding strength, excellent sealing performance, and optimal material condition under overall low-temperature conditions.

[0031] The synergistic effect of the above-mentioned technical steps enables the prepared float to exhibit superior comprehensive performance. The bonding strength is significantly improved compared to traditional processes, and the sealing reliability achieves zero pressure decay. After long-term fatigue cycling and media immersion, the performance degradation rate is extremely low. This technical solution completely solves the industry's persistent problems such as easy peeling of the interface, easy seal failure, and poor durability of traditional floats, providing a brand-new systematic solution for the preparation of highly reliable and long-life float products. Detailed Implementation

[0032] 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 are described clearly and completely. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0033] The raw materials used in the embodiments and comparative examples of this invention are industrial grade. Other raw materials are shown below: The fiber fabric is a blend of nylon 66 and aramid 1414; its areal density is 200 g / m². 2 Thickness 0.3mm; Plain weave structure.

[0034] Stearic acid: Type 200, Grade 1.

[0035] Natural rubber: Smoked sheet rubber RSS3, Mooney viscosity ML1+4 (100℃) 60 Chloroprene rubber: CR2442 (general purpose, medium crystallization rate) Silica: Precipitated silica, specific surface area 150-200 m² 2 / g The organic solvent (for adhesive paste) is a toluene:xylene mixture in a 1:1 volume ratio. In the embodiments and comparative examples of this invention, the clean environment has a cleanliness level of ≥100,000.

[0036] The dimensions of the floats prepared in the embodiments and comparative examples of the present invention are shown in Table 1 below: Table 1

[0037] Example 1 A method for preparing a high-performance float based on multi-technology synergy specifically includes the following steps: S1. The fiber fabric is immersed in a 5wt% sodium hydroxide solution at 50℃ with a bath ratio of 1g:20mL, and ultrasonically treated (ultrasonic power of 200W, ultrasonic frequency of 25kHz) for 10 minutes; then rinsed with deionized water until neutral, and dried with hot air at 80℃ to constant weight; the dried fiber fabric is sprayed with a silane coupling agent solution (silane coupling agent solution is KH-550 ethanol solution, KH-550 content is 1wt%) on the surface (spray gun air pressure of 0.5MPa, spraying distance of 20cm, gun speed of 0.3m / s), and then dried and cured at 120℃ for 5 minutes to obtain the pretreated fabric; S2. Weigh the rubber compound according to the formula, mix it in a two-stage internal mixer, and then sheet it out. Let it cure for 24 hours at a curing temperature of 23±2℃ and a humidity of 50±5% to obtain the rubber sheet. Dissolve the same rubber compound in an organic solvent to prepare a 20wt% adhesive paste, spray it onto the surface of the rubber sheet, and let it dry in a clean environment for 15 minutes. The dry adhesive adhesion after brushing is 6±2g / m². 2 The pre-treated film is obtained; The rubber compound specifically includes the following raw materials by weight: 100 parts natural rubber, 20 parts chloroprene rubber, 4 parts resorcinol resin, 2 parts formaldehyde donor (hexamethylenetetramine), 25 parts silica, 5 parts activator (zinc oxide), 1 part stearic acid, 2 parts accelerator (the accelerator is obtained by mixing accelerator M and accelerator DM in a mass ratio of 2:1), 2 parts anti-aging agent (the anti-aging agent is obtained by mixing RD and 4010NA in a mass ratio of 2:1), and 3 parts tackifying resin (C5 petroleum resin, softening point 100-120℃). The two-stage mixed practice specifically includes the following steps: A1. Put natural rubber and chloroprene rubber into a mixer and masticate for 30 seconds. Then add 2 / 3 of the formula amount of resorcinol resin, activator, stearic acid, anti-aging agent and the full amount of formula amount of silica. Sweep up the powder to ensure that all of it falls into the mixing chamber. Set the top pressure to 0.6MPa and mix at a speed of 80rpm until the system temperature rises to 150℃. Discharge the rubber and let it cool and stand for 24 hours to obtain a first-stage rubber. A2. Add a section of adhesive to the internal mixer and control the mixing temperature within the range of 90-100℃. Then add the remaining 1 / 3 of the formula amount of resorcinol resin, activator, stearic acid, and anti-aging agent and mix at a rate of 60 rpm for 3 minutes. Next, add the formaldehyde donor, accelerator, and tackifying resin according to the formula amount. Set the top tamper pressure to 0.3MPa and continue mixing. Control the discharge temperature to ≤110℃. Discharge the adhesive immediately after 60 seconds. After discharge, perform triangular wrapping 8 times under the condition of roller temperature <50℃ for further homogenization and then sheet out. Set the sheet thickness to 1.0mm.

[0038] S3. Precisely bond the pretreated film and pretreated fabric in a clean environment, and roll press to remove air bubbles to obtain the pre-shaped float material. Specifically, the air bubble removal is achieved by rolling at least three times from the center to the edge using a three-roll calender. The speed ratio of the upper, middle, and lower rolls is 10m / min:11.5m / min:13.5m / min. The temperature of the upper roll is set to 40℃, the temperature of the middle roll is set to 45℃, and the temperature of the lower roll is set to 50℃. The ambient temperature is controlled at 25℃ and the humidity is <60%.

[0039] S4. Place the pre-shaped float material into the mold, apply differentiated pressure to the long side, short side, and air inlet / outlet through the segmented mold, and start the timed vulcanization. The specific operation is as follows: first apply a pressure of 0.8MPa to the whole, preheat for 10 minutes to allow the rubber material to flow and fill, and then vulcanize according to the following parameters: long side vulcanization pressure 1.3MPa, vulcanization time 110 minutes, vulcanization temperature 85℃; short side vulcanization pressure 1.0MPa, vulcanization time 100 minutes, vulcanization temperature 85℃; air inlet and air outlet vulcanization pressure 1.6MPa, vulcanization time 120 minutes, vulcanization temperature 85℃.

[0040] After vulcanization, the material is naturally cooled to below 60°C before demolding. After mechanical trimming, the float is obtained.

[0041] Example 2 A method for preparing a high-performance float based on multi-technology synergy specifically includes the following steps: S1. The fiber fabric is immersed in a 5wt% sodium hydroxide solution at 50℃ with a bath ratio of 1g:20mL, and ultrasonically treated (ultrasonic power of 250W, ultrasonic frequency of 30kHz) for 10 minutes; then rinsed with deionized water until neutral, and dried with hot air at 80℃ to constant weight; the dried fiber fabric is sprayed with a silane coupling agent solution (silane coupling agent solution is KH-550 ethanol solution, KH-550 content is 2wt%) on the surface (spray gun air pressure of 0.5MPa, spraying distance of 20cm, gun speed of 0.3m / s), and then dried and cured at 120℃ for 5 minutes to obtain the pretreated fabric; S2. Weigh the rubber compound according to the formula, mix it in a two-stage internal mixer, and then sheet it out. Let it cure for 24 hours at a curing temperature of 23±2℃ and a humidity of 50±5% to obtain the rubber sheet. Dissolve the same rubber compound in an organic solvent to prepare a 20wt% adhesive paste, spray it onto the surface of the rubber sheet, and let it dry in a clean environment for 15 minutes. The dry adhesive adhesion after brushing is 6±2g / m². 2 The pre-treated film is obtained; The rubber compound specifically includes the following raw materials by weight: 100 parts natural rubber, 25 parts chloroprene rubber, 5 parts resorcinol resin, 3 parts formaldehyde donor (hexamethylenetetramine), 30 parts silica, 6 parts activator (zinc oxide), 1.5 parts stearic acid, 2 parts accelerator (the accelerator is obtained by mixing accelerator M and accelerator DM in a mass ratio of 3:1), 2 parts anti-aging agent (the anti-aging agent is obtained by mixing RD and 4010NA in a mass ratio of 3:1), and 4 parts tackifying resin (C5 petroleum resin, softening point 100-120℃). The two-stage mixed practice specifically includes the following steps: A1. Put natural rubber and chloroprene rubber into a mixer and masticate for 30 seconds. Then add 2 / 3 of the formula amount of resorcinol resin, activator, stearic acid, anti-aging agent and the full amount of formula amount of silica. Sweep up the powder to ensure that all of it falls into the mixing chamber. Set the top pressure to 0.8MPa and mix at a speed of 80rpm until the system temperature rises to 150℃. Discharge the rubber and let it cool and stand for 24 hours to obtain a first-stage rubber. A2. Add a section of adhesive to the internal mixer and control the mixing temperature within the range of 90-100℃. Then add the remaining 1 / 3 of the formula amount of resorcinol resin, activator, stearic acid, and anti-aging agent and mix at a rate of 60 rpm for 3 minutes. Next, add the formaldehyde donor, accelerator, and tackifying resin according to the formula amount. Set the top tamper pressure to 0.4 MPa and continue mixing. Control the discharge temperature to ≤110℃. Discharge the adhesive immediately after 60 seconds. After discharge, perform triangular wrapping 8 times under the condition of roller temperature <50℃ for further homogenization and then sheet out. Set the sheet thickness to 1.0 mm.

[0042] S3. Precisely bond the pretreated film and pretreated fabric in a clean environment, and roll press to remove air bubbles to obtain the pre-shaped float material. Specifically, the air bubble removal is achieved by rolling at least three times from the center to the edge using a three-roll calender. The speed ratio of the upper, middle, and lower rolls is 10 m / min:11.5 m / min:13.5 m / min. The temperature of the upper roll is set to 45℃, the middle roll to 50℃, and the lower roll to 55℃. The ambient temperature is controlled at 25℃ and the humidity is <60%.

[0043] S4. Place the pre-shaped float material into the mold, apply differentiated pressure to the long side, short side, and air inlet / outlet through the segmented mold, and start the timed vulcanization. The specific operation is as follows: first apply a pressure of 0.8MPa to the whole, preheat for 10 minutes to allow the rubber material to flow and fill, and then vulcanize according to the following parameters: long side vulcanization pressure 1.4MPa, vulcanization time 120 minutes, vulcanization temperature 90℃; short side vulcanization pressure 1.1MPa, vulcanization time 110 minutes, vulcanization temperature 90℃; air inlet and air outlet vulcanization pressure 1.7MPa, vulcanization time 140 minutes, vulcanization temperature 90℃.

[0044] After vulcanization, the material is naturally cooled to below 60°C before demolding. After mechanical trimming, the float is obtained.

[0045] Example 3 A method for preparing a high-performance float based on multi-technology synergy specifically includes the following steps: S1. The fiber fabric is immersed in a 5wt% sodium hydroxide solution at 50℃ with a liquor ratio of 1g:20mL, and ultrasonically treated (ultrasonic power of 300W, ultrasonic frequency of 40kHz) for 10 minutes; then rinsed with deionized water until neutral, and dried with hot air at 80℃ to constant weight; the dried fiber fabric is sprayed with a silane coupling agent solution (silane coupling agent solution is KH-550 ethanol solution, KH-550 content is 2wt%) on the surface (spray gun air pressure 0.5MPa, spraying distance of 20cm, gun speed of 0.3m / s), and then dried and cured at 120℃ for 5 minutes to obtain the pretreated fabric; S2. Weigh the rubber compound according to the formula, mix it in a two-stage internal mixer, and then sheet it out. Let it cure for 24 hours at a curing temperature of 23±2℃ and a humidity of 50±5% to obtain the rubber sheet. Dissolve the same rubber compound in an organic solvent to prepare a 20wt% adhesive paste, spray it onto the surface of the rubber sheet, and let it dry in a clean environment for 15 minutes. The dry adhesive adhesion after brushing is 6±2g / m². 2 The pre-treated film is obtained; The rubber compound specifically includes the following raw materials by weight: 100 parts natural rubber, 30 parts chloroprene rubber, 6 parts resorcinol resin, 3 parts formaldehyde donor (hexamethylenetetramine), 35 parts silica, 6 parts activator (zinc oxide), 1.5 parts stearic acid, 3 parts accelerator (the accelerator is obtained by mixing accelerator M and accelerator DM in a mass ratio of 3:1), 3 parts anti-aging agent (the anti-aging agent is obtained by mixing RD and 4010NA in a mass ratio of 3:1), and 5 parts tackifying resin (C5 petroleum resin, softening point 100-120℃). The two-stage mixed practice specifically includes the following steps: A1. Put natural rubber and chloroprene rubber into a mixer and masticate for 30 seconds. Then add 2 / 3 of the formula amount of resorcinol resin, activator, stearic acid, anti-aging agent and the full amount of formula amount of silica. Sweep up the powder to ensure that all of it falls into the mixing chamber. Set the top pressure to 0.8MPa and mix at a speed of 80rpm until the system temperature rises to 150℃. Discharge the rubber and let it cool and stand for 24 hours to obtain a first-stage rubber. A2. Add a section of adhesive to the internal mixer and control the mixing temperature within the range of 90-100℃. Then add the remaining 1 / 3 of the formula amount of resorcinol resin, activator, stearic acid, and anti-aging agent and mix at a rate of 60 rpm for 3 minutes. Next, add the formaldehyde donor, accelerator, and tackifying resin according to the formula amount. Set the top tamper pressure to 0.5MPa and continue mixing. Control the discharge temperature to ≤110℃. Discharge the adhesive immediately after 60 seconds. After discharge, perform triangular wrapping 8 times under the condition of roller temperature <50℃ for further homogenization and then sheet out. Set the sheet thickness to 1.0mm.

[0046] S3. Precisely bond the pretreated film and pretreated fabric in a clean environment, and roll press to remove air bubbles to obtain the pre-shaped float material. Specifically, the air bubble removal is achieved by using a three-roll calender to roll from the center to the edge at least three times. The speed ratio of the upper, middle, and lower rolls is 10m / min:11.5m / min:13.5m / min. The temperature of the upper roll is set to 50℃, the temperature of the middle roll is set to 55℃, and the temperature of the lower roll is set to 60℃. The ambient temperature is controlled at 25℃ and the humidity is <60%.

[0047] S4. Place the pre-shaped float material into the mold, apply differentiated pressure to the long side, short side, and air inlet / outlet through the segmented mold, and start the timed vulcanization. The specific operation is as follows: first apply a pressure of 0.8MPa to the whole, preheat for 10 minutes to allow the rubber material to flow and fill, and then vulcanize according to the following parameters: long side vulcanization pressure 1.4MPa, vulcanization time 150 minutes, vulcanization temperature 95℃; short side vulcanization pressure 1.1MPa, vulcanization time 130 minutes, vulcanization temperature 95℃; air inlet and air outlet vulcanization pressure 1.7MPa, vulcanization time 160 minutes, vulcanization temperature 95℃.

[0048] After vulcanization, the material is naturally cooled to below 60°C before demolding. After mechanical trimming, the float is obtained.

[0049] Comparative Example 1 The difference between this comparative example and Example 2 is that in step S2, the resorcinol system is not used in the rubber compound; instead, natural rubber is used to replace the resorcinol resin and formaldehyde donor. Specifically, in this comparative example, the rubber compound comprises the following parts by weight: 108 parts natural rubber, 25 parts chloroprene rubber, 30 parts silica, 6 parts activator (zinc oxide), 1.5 parts stearic acid, 2 parts accelerator (the accelerator is obtained by mixing accelerator M and accelerator DM in a 3:1 mass ratio), 2 parts anti-aging agent (the anti-aging agent is obtained by mixing RD and 4010NA in a 3:1 mass ratio), and 4 parts tackifying resin (C5 petroleum resin, softening point 100-120℃).

[0050] Comparative Example 2 The difference between this comparative example and Example 2 is that in step S2, the rubber compounding is performed in a single-stage mixing process, meaning all raw materials are added and mixed at once. Specifically, in this comparative example, the film is prepared through the following steps: Weigh the rubber compound according to the formula, mix it in an internal mixer, and then sheet it out. Let it stand for 24 hours to cure at a temperature of 23±2℃ and a humidity of 50±5% to obtain the rubber sheet. The mixing process includes the following steps: Natural rubber and chloroprene rubber were put into a mixer and plasticized for 30 seconds. Then, resorcinol resin, activator, stearic acid, anti-aging agent and fumed silica were added according to the formula. The powder was swept away to ensure that all of it fell into the mixing chamber. The mixture was mixed at 60 rpm for 3 minutes. Then, formaldehyde donor, accelerator and tackifying resin were added according to the formula. The top pressure was set to 0.8 MPa and the mixture was mixed at 80 rpm until the system temperature rose to 150°C. After the mixture was discharged, it was rolled into triangular bundles 8 times under the condition that the roller temperature was <50°C. After cooling and standing for 24 hours, it was further homogenized and then sheeted. The sheet thickness was set to 1.0 mm.

[0051] Comparative Example 3 The difference between this comparative example and Example 2 is that in step S3, instead of using a three-roll calender, a simple rolling process using ordinary rollers is adopted, with the roller speed set at 11.5 m / min and the roller temperature at 50°C.

[0052] Comparative Example 4 The difference between this comparative example and Example 2 is that in step S4, vulcanization does not use segmented pressure, but instead uses a uniform pressure (1.3 MPa) and time (120 minutes). Specifically, the vulcanization operation in step S4 of this comparative example is as follows: First, apply a pressure of 0.8 MPa to the whole and preheat for 10 minutes to allow the rubber compound to flow and fill. Then, vulcanize the long side, short side, and air inlet and outlet at a vulcanization pressure of 1.3 MPa for 120 minutes, and set the vulcanization temperature to 90℃.

[0053] The performance of the floats prepared in the examples and comparative examples is now being tested. The specific test methods are as follows: Adhesion strength test: Refer to the peel strength test method described in GB / T532-2008 "Determination of Adhesion Strength between Vulcanized Rubber or Thermoplastic Rubber and Fabric". Peel the fabric (main adhesive sheet: rectangular sheet, 860mm×310mm) from the rubber layer at 180° and test the peel strength, unit: kN / m. The test speed is set to 100mm / min.

[0054] Sealing performance test: Inflate the finished float to 0.5MPa, maintain the pressure for 30 minutes, record the pressure drop value, and judge the sealing performance of the sample by the percentage of pressure loss.

[0055] Aging resistance test: A) 500 inflation / deflation cycles: Inflate the finished float to 0.5 MPa and then deflate completely, which is considered one cycle. Repeat 500 times. Test the bond strength (peel strength) and sealing performance of the float before and after the cycles, and calculate the performance degradation rate. Degradation rate = (initial value - value after cycle) / initial value × 100%.

[0056] B) The finished floatation bladder was immersed in a 3.5wt% NaCl solution to simulate seawater, with the temperature controlled at 25±2℃, for 300 days.

[0057] The specific test results are shown in Tables 2 and 3 below.

[0058] Table 2 Bond strength and sealing performance tests

[0059] Table 3 Aging resistance test

[0060] As shown in Tables 2 and 3, the samples obtained in the examples outperformed those in the comparative examples, with the sample in Example 2 exhibiting the best performance. In Comparative Example 1, the removal of the meta-methyl system resulted in a sharp decrease in bond strength, a significant increase in pressure decay rate, and a significant deterioration in aging resistance. This indicates that the meta-methyl resin system is a key element in forming a high-strength chemically bonded interface; its absence makes the interface the weakest link, leading to severely compromised sealing and durability of the float.

[0061] In Comparative Example 2, the use of a single-stage mixing method resulted in reduced bond strength, and a significant decrease in fatigue resistance and seawater resistance. Single-stage mixing cannot ensure sufficient dispersion of fillers such as silica, and the vulcanization system added at high temperatures may partially react prematurely, leading to poor uniformity of the rubber compound, interfacial stress concentration, and consequently affecting overall reliability.

[0062] In Comparative Example 3, using ordinary roll-pressed bonding materials resulted in low bond strength and poor sealing of the final product. Simple roll pressing without controlling temperature and speed cannot effectively eliminate interfacial air bubbles or achieve sufficient wetting of the fabric by the adhesive, leaving microscopic defects. These defects gradually expand during cyclic inflation / deflation and media immersion, accelerating performance degradation.

[0063] In Comparative Example 4, after vulcanization with uniform pressure and time, all properties were inferior to those of Example 2. Insufficient pressure on the long sides resulted in weak adhesion, while excessive pressure on the short sides caused excessive flow of the adhesive. Insufficient pressure also led to poor sealing of the air inlets and outlets. This confirms that segmented pressure vulcanization can precisely meet the stress requirements of different parts and is key to obtaining uniform and dense products.

[0064] It should be noted that, in this document, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such a process, method, article, or apparatus. Unless otherwise specified, an element defined by the phrase "comprising one..." does not exclude the presence of other identical elements in the process, method, article, or apparatus that includes said element.

[0065] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

[0066] Those skilled in the art should understand that the above descriptions are merely several specific embodiments of the present invention, and not all embodiments.

Claims

1. A method for preparing a high-performance floating capsule based on multi-technology cooperation, characterized in that, The preparation steps include the following: S1. After alkaline cleaning of the fiber fabric, it is washed with water, dried, modified with a silane coupling agent, and then dried to obtain the pretreated fabric. S2. Weigh the rubber compound according to the formula, mix it in two stages in an internal mixer, and then sheet it out. Let it stand for curing for at least 24 hours to obtain the film. Dissolve the same rubber compound in an organic solvent to prepare a 15-25wt% rubber paste, spray it on the surface of the film, and let it dry for 10-15 minutes to obtain the pretreated film. S3. Lay the pre-treated film and the pre-treated fabric together, roll them to remove air bubbles, and obtain the pre-shaped float material. S4. Place the pre-shaped float material into the mold, apply differentiated pressure to the long side, short side, and air inlet / outlet through the segmented mold, and start timing vulcanization. After vulcanization is completed, allow it to cool naturally and demold to obtain the float.

2. The method of claim 1, wherein the method comprises the steps of: The pretreated fabric is prepared by the following steps: The fiber fabric is immersed in an alkaline washing solution at 50-60℃ and ultrasonically treated for 5-10 minutes; then rinsed until neutral and dried; the dried fiber fabric is sprayed with a silane coupling agent solution, and then dried and cured to obtain the pretreated fabric.

3. The method for preparing a high-performance float based on multi-technology synergy as described in claim 2, characterized in that, The specific parameters for the spraying are as follows: spray gun air pressure 0.3-0.5 MPa, spraying distance 15-25 cm, gun travel speed 0.3-0.6 m / s, and target dry film coating amount 0.5-1.5 g / m. 2 .

4. The method for preparing a high-performance float based on multi-technology synergy as described in claim 1, characterized in that, In step S2, the adhesive material specifically comprises the following parts by weight of raw materials: 100 parts natural rubber, 10-50 parts chloroprene rubber, 1-10 parts resorcinol resin, 1-10 parts formaldehyde donor, 25-35 parts silica, 5-6 parts activator, 1-1.5 parts stearic acid, 2-3 parts accelerator, 2-3 parts anti-aging agent, and 3-5 parts tackifying resin.

5. The method of claim 4, wherein the high performance floating capsule is prepared based on multi-technology cooperation. The accelerator is obtained by mixing accelerator M and accelerator DM in a mass ratio of (2-3):

1.

6. The method of claim 4, wherein the high performance floating capsule is prepared based on multi-technology cooperation. The anti-aging agent is obtained by mixing RD and 4010NA in a mass ratio of (2-3):

1.

7. The method of claim 4, wherein the high performance floating capsule is prepared based on multi-technology cooperation. In step S2, the two-stage mixing specifically includes the following steps: A1. Put natural rubber and chloroprene rubber into a mixer for plasticizing. Then add 2 / 3 of the formula amount of resorcinol resin, activator, stearic acid, anti-aging agent and the full amount of formula amount of fumed silica. Set the top plug pressure to 0.6-0.8MPa and mix at a rate of 60-80rpm until the system temperature rises to 145-155℃. Discharge the rubber and let it cool and stand for 4-24 hours to obtain a first-stage rubber. A2. Put a section of glue into an internal mixer and control the mixing temperature within the range of 90-100℃. Then add the remaining 1 / 3 of the formula amount of resorcinol resin, activator, stearic acid, and anti-aging agent and mix. Then add the formaldehyde donor, accelerator, and tackifying resin according to the formula amount. Continue mixing and then discharge the glue. After discharging the glue, make triangular wraps 5-8 times to further homogenize before sheeting.

8. The method of claim 1, wherein the high performance floating capsule is prepared based on multi-technology cooperation. In step S3, the rolling process specifically employs a three-roll calender to roll the rollers from the center to the edge at least three times. The speed ratio of the upper, middle, and lower rollers is 1:1.1-1.2:1.3-1.

4. The temperature of the upper roller is set to 40-50℃, the temperature of the middle roller is set to 45-55℃, and the temperature of the lower roller is set to 50-60℃. The ambient temperature is controlled at 20-28℃, and the humidity is <60%.

9. The method of claim 1, wherein the high performance floating capsule is prepared based on multi-technology cooperation. In step S4, the vulcanization specifically involves: first, applying a pressure of 0.8 MPa to the entire material and preheating for 10 minutes to allow the rubber compound to flow and fill; then, vulcanizing according to the following parameters: long side vulcanization pressure 1.3-1.4 MPa, vulcanization time 110-150 minutes, vulcanization temperature 85-95℃; short side vulcanization pressure 1.0-1.1 MPa, vulcanization time 100-130 minutes, vulcanization temperature 85-95℃; and inlet and outlet vulcanization pressure 1.6-1.7 MPa, vulcanization time 120-160 minutes, vulcanization temperature 85-95℃.

10. A float prepared by a method for preparing a high-performance float based on multi-technology synergy according to any one of claims 1-9.