Corrosion-resistant flame-retardant cloth and preparation method thereof

Abstract

The invention discloses corrosion-resistant flame-retardant cloth and a preparation method thereof, and belongs to the technical field of flame-retardant cloth preparation. The preparation method of the corrosion-resistant flame-retardant cloth comprises the following steps: step 1, carrying out alkali treatment on aramid fiber cloth to obtain pretreated aramid fibers; and 2, adding a flame-retardant complexing agent and a corrosion-resistant agent into novolac epoxy resin containing a light curing agent, performing ultrasonic stirring to obtain an impregnation liquid, adding the pretreated aramid fiber into the impregnation liquid, and performing soaking, curing, heat treatment and water washing to obtain the corrosion-resistant flame-retardant cloth. The flame-retardant cloth prepared by the method has excellent flame retardance and corrosion resistance.

Description

Technical Field

[0001] The present invention belongs to the technical field of flame-retardant cloth preparation, and in particular relates to a corrosion-resistant flame-retardant cloth and a preparation method thereof. Background Art

[0002] In the fields of industrial safety, public facility protection, and special operating environments, the demand for multifunctional protective properties of materials is becoming increasingly prominent. Among them, corrosion-resistant flame-retardant fabrics, as key materials that combine flame retardancy with chemical corrosion resistance, have seen their performance optimization become a key area of technological breakthrough in the industry. Traditional flame-retardant fabrics have significant limitations when dealing with complex environments: on the one hand, most flame-retardant materials achieve fire resistance by adding halogen compounds or phosphorus-based flame retardants, but these chemicals tend to release toxic fumes during high-temperature combustion and are prone to structural degradation when exposed to acidic and alkaline environments for long periods, leading to a decrease in flame retardant properties. On the other hand, while conventional corrosion-resistant coatings can improve the fabric's resistance to chemical corrosion, they often come at the expense of flame retardancy.

[0003] Patent CN114263046B discloses a corrosion-resistant blended fabric and a preparation method thereof, comprising a base fabric layer and a corrosion-resistant functional layer provided on the surface of the base fabric layer; the base fabric layer is woven from a blended yarn made by blending PBT elastic fiber T300, white polyester-based coconut charcoal fiber, and chitosan fiber; the corrosion-resistant functional layer comprises the following components by weight: 30-40 parts of epoxy-containing hyperbranched polyborosiloxane, 2-4 parts of nano-boron fiber, 1-2 parts of fluorinated graphene, 2-4 parts of 2,4-diamino-6-diallylamino-1,3,5-triazine, 2-4 parts of 2-[3-(2H-benzotriazole-2-yl)-4-hydroxyphenyl]ethyl-2-methacrylate, 3-5 parts of vinyltrimethoxysilane, 8-10 parts of N-(4-cyano-3-trifluoromethylphenyl)methacrylamide, and 0.07-0.1 parts of a photoinitiator. The blended fabric prepared by the above method has excellent corrosion resistance, good mechanical properties and flame retardancy. However, the corrosion resistance and flame retardancy of the flame retardant cloth prepared by this method still have room for improvement. Summary of the Invention

[0004] The object of the present invention is to provide a corrosion-resistant flame-retardant cloth and a preparation method thereof, so as to solve the technical problem that the flame-retardant cloth in the prior art has poor corrosion resistance and flame retardancy.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions:

[0006] The present invention provides a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0007] Step 1: treating the aramid fiber cloth with alkali to obtain pretreated aramid fiber;

[0008] Step 2: adding the flame retardant composite and the corrosion resistant agent to the phenolic epoxy resin containing the light curing agent, ultrasonically stirring to obtain an impregnation solution, adding the pretreated aramid fiber to the impregnation solution for immersion, curing, heat treatment, and water washing to obtain a corrosion-resistant flame retardant cloth.

[0009] Preferably, in the step 1, a 0.5 mol / L sodium hydroxide solution is used for the alkali treatment process, and in the step 2, the amount ratio of the flame retardant composite, the corrosion resisting agent and the phenolic epoxy resin is (12-25) g: (11-18) g: (150-220) mL.

[0010] Preferably, the method for preparing the flame retardant composite comprises the following steps:

[0011] Q1: Octamethylcyclotetrasiloxane and γ-aminopropylmethyldimethoxysilane were added to a container, heated and stirred to mix, potassium hydroxide was added, and the temperature was continued to react, and then hexamethyldisiloxane was added to continue the reaction. After the reaction was completed, rotary evaporation was performed and the pH was adjusted to neutral to obtain compound 1;

[0012] Q2: Add diphenyl chlorophosphate to a container, then add tetrahydrofuran, stir to dissolve, then mix compound 1 with triethylamine and place in a funnel, add dropwise to the container under low temperature environment, control the addition time, and after the addition is completed, heat to room temperature for reaction. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0013] In the above process, the synthetic reaction formula of the flame retardant composite is as follows:

[0014]

[0015] Preferably, in Q1, the amount ratio of octamethylcyclotetrasiloxane, γ-aminopropylmethyldimethoxysilane, potassium hydroxide and hexamethyldisiloxane is (1.68-2.01) g: (1.01-1.35) g: (0.1-0.15) g: (0.88-1.14) g, the heating and stirring temperature is 80-85°C, the heating reaction temperature is continued to be 100-105°C, the reaction time is 6-8h, and hexamethyldisiloxane is added and the reaction is continued for 1-2h.

[0016] Preferably, in Q2, the usage ratio of diphenyl chlorophosphate, tetrahydrofuran, compound 1 and triethylamine is (123.45-143.52) g: (700-900) mL: (213.23-222.57) g: (52.11-59.83) g, the low temperature environment temperature is 0-5°C, the dropwise addition time is 3-5 h, and the reaction time at room temperature is 10-12 h.

[0017] Preferably, the method for preparing the corrosion resistant agent comprises the following steps:

[0018] S1: Under argon protection, 4,4-difluorobenzophenone, 4A molecular sieve, aniline and toluene are added to a container, and the temperature is increased during mechanical stirring. The temperature is increased and stirred for reaction. After the reaction is completed, the mixture is cooled, filtered, rotary evaporated, recrystallized, and dried to obtain a monomer;

[0019] S2: Add o-cresolphthalein, monomer, potassium carbonate, toluene and N-methylpyrrolidone into a container, introduce nitrogen, heat with stirring and reflux, discharge the toluene in the water separator in batches, raise the temperature to react, precipitate after the reaction, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0020] In the above process, the synthetic reaction formula of the corrosion resistant agent is as follows:

[0021]

[0022] The results of mass spectrometry analysis of the monomer were: m / z: 293.10 (100.0%), 294.10 (20.9%), 295.11 (2.0%).

[0023] Preferably, in S1, the amount ratio of 4,4-difluorobenzophenone, 4A molecular sieve, aniline and toluene is (20.02-22.64) g: (45-55) g: (12.2-14.6) mL: (70-90) mL, the reaction temperature is 155-165 ° C., the reaction time is 20-24 h, and the mixture is added to methanol for recrystallization. The drying temperature is 60-70 ° C. and the time is 10-12 h.

[0024] Preferably, in S2, the amount ratio of o-cresolphthalein, monomer, potassium carbonate, toluene and N-methylpyrrolidone is (20-30) g: (11-13.5) g: (14.2-18.4) g: (70-75) mL: (200-234) mL, the heating and stirring reflux temperature is 140-150° C., the reflux time is 1-2 h, the heating reaction temperature is 180-185° C., and the reaction time is 3-6 h.

[0025] The corrosion-resistant flame-retardant cloth is prepared by the above-mentioned preparation method.

[0026] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0027] 1. The flame retardant composite and corrosion resistant agent prepared in the present invention are applied to the flame retardant cloth, which can effectively improve the flame retardant and corrosion resistance of the flame retardant cloth and extend the service life of the flame retardant cloth.

[0028] 2. The present invention connects the organic silicon structural unit and the nitrogen-phosphorus flame retardant structural unit through chemical bonds to obtain a flame retardant composite. Applying it to flame retardant cloth can effectively improve its flame retardant properties and corrosion resistance. The phosphorus element contained in it promotes carbonization, and the nitrogen element decomposes to produce non-combustible gas to dilute the combustible material. The organic silicon chain segments migrate to the surface at high temperature to form a strong, dense, and heat-insulating silicon-carbon composite protective layer, which effectively isolates heat and oxygen, inhibits volatiles, and synergistically improves the flame retardant effect; the organic silicon main chain contained in it gives the cloth surface strong hydrophobicity, effectively repels water, oil and polar liquids, blocks the penetration of water-soluble corrosive media, delays the corrosion process, and improves the corrosion resistance effect.

[0029] 3. The present invention applies the prepared corrosion resistance agent to flame-retardant cloth, which can effectively improve its corrosion resistance. The phenolphthalein carbene structure contained in it has a rigid planar large conjugated system and steric hindrance, which can effectively shield the erosion of chemical media. At the same time, the high-energy ether bond contained in it can also resist acid and alkali hydrolysis, thereby improving the corrosion resistance of the flame-retardant cloth. DETAILED DESCRIPTION

[0030] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0031] Example 1: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0032] Q1: 1.83 g of octamethylcyclotetrasiloxane and 1.18 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, and then 0.12 g of potassium hydroxide was added. The temperature was then continued to rise to 100°C and the reaction was continued for 8 h. Then, 1.01 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0033] Q2: Add 133.41g of diphenyl chlorophosphate to a container, then add 800mL of tetrahydrofuran, stir to dissolve, then mix 217.71g of compound 1 and 55.91g of triethylamine and place in a funnel. Add dropwise to the container at 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0034] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0035] S1: Under argon protection, 21.33 g of 4,4-difluorobenzophenone, 50 g of 4A molecular sieve, 13.4 mL of aniline, and 80 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0036] S2: Add 25g of o-cresolphthalein, 12.7g of monomer, 16.3g of potassium carbonate, 72.5mL of toluene and 217mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0037] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0038] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0039] Step 2: Add 18.5g of flame retardant composite and 14.5g of corrosion resistant agent to 185mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain a corrosion-resistant flame retardant cloth.

[0040] Example 2: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0041] Q1: 1.68 g of octamethylcyclotetrasiloxane and 1.01 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, 0.1 g of potassium hydroxide was added, and the temperature was continued to rise to 100°C for 8 h. Then, 0.88 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0042] Q2: Add 123.45g of diphenyl chlorophosphate to a container, then add 700mL of tetrahydrofuran, stir to dissolve, then mix 213.23g of compound 1 with 52.11g of triethylamine and place in a funnel. Add dropwise to the container at 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0043] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0044] S1: Under argon protection, 20.02 g of 4,4-difluorobenzophenone, 55 g of 4A molecular sieve, 12.2 mL of aniline, and 90 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0045] S2: Add 30g of o-cresolphthalein, 13.5g of monomer, 14.2g of potassium carbonate, 75mL of toluene and 200mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0046] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0047] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0048] Step 2: Add 12g of flame retardant composite and 18g of corrosion resistant agent to 150mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain corrosion-resistant flame retardant cloth.

[0049] Example 3: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0050] Q1: 2.01 g of octamethylcyclotetrasiloxane and 1.35 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, 0.15 g of potassium hydroxide was added, and the temperature was continued to rise to 100°C for 8 h. Then, 1.14 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0051] Q2: Add 143.52g of diphenyl chlorophosphate to a container, then add 900mL of tetrahydrofuran, stir to dissolve, then mix 222.57g of compound 1 and 59.83g of triethylamine and place in a funnel. Add dropwise to the container at 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0052] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0053] S1: Under argon protection, 22.64 g of 4,4-difluorobenzophenone, 45 g of 4A molecular sieve, 14.6 mL of aniline, and 70 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0054] S2: Add 20g of o-cresolphthalein, 11g of monomer, 18.4g of potassium carbonate, 70mL of toluene and 234mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0055] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0056] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0057] Step 2: Add 25g of flame retardant composite and 11g of corrosion resistant agent to 220mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain corrosion-resistant flame retardant cloth.

[0058] Example 4: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0059] Q1: 1.72 g of octamethylcyclotetrasiloxane and 1.17 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, 0.11 g of potassium hydroxide was added, and the temperature was continued to rise to 100°C for 8 h. Then, 0.92 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0060] Q2: Add 128.43g of diphenyl chlorophosphate to a container, then add 750mL of tetrahydrofuran, stir to dissolve, then mix 215.18g of compound 1 and 53.91g of triethylamine and place in a funnel. Add dropwise to the container at a low temperature of 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0061] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0062] S1: Under argon protection, 20.58 g of 4,4-difluorobenzophenone, 48 g of 4A molecular sieve, 13.8 mL of aniline, and 75 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0063] S2: Add 22g of o-cresolphthalein, 11.8g of monomer, 15.1g of potassium carbonate, 71mL of toluene and 207mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0064] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0065] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0066] Step 2: Add 15g of flame retardant composite and 12g of corrosion resistant agent to 160mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain corrosion-resistant flame retardant cloth.

[0067] Comparative Example 5: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0068] Q1: 1.91 g of octamethylcyclotetrasiloxane and 1.24 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, and then 0.14 g of potassium hydroxide was added. The temperature was then continued to rise to 100°C and the reaction was continued for 8 h. Then, 1.08 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0069] Q2: Add 138.48g of diphenyl chlorophosphate to a container, then add 850mL of tetrahydrofuran, stir to dissolve, then mix 219.91g of compound 1 and 58.71g of triethylamine and place in a funnel. Add dropwise to the container at a low temperature of 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0070] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0071] S1: Under argon protection, 21.87 g of 4,4-difluorobenzophenone, 52 g of 4A molecular sieve, 14.2 mL of aniline, and 85 mL of toluene were added to a container. The temperature was raised to 160°C during mechanical stirring and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70°C for 12 h to obtain a monomer.

[0072] S2: Add 28g of o-cresolphthalein, 13.1g of monomer, 17.2g of potassium carbonate, 74mL of toluene and 228mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0073] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0074] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0075] Step 2: Add 23g of flame retardant composite and 16g of corrosion resistant agent to 200mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain corrosion-resistant flame retardant cloth.

[0076] Example 6: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0077] Q1: 1.75 g of octamethylcyclotetrasiloxane and 1.07 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, 0.12 g of potassium hydroxide was added, and the temperature was continued to rise to 100°C for 8 h. Then, 0.91 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0078] Q2: Add 125.55g of diphenyl chlorophosphate to a container, then add 780mL of tetrahydrofuran, stir to dissolve, then mix 214.53g of compound 1 and 54.12g of triethylamine and place in a funnel. Add dropwise to the container at a low temperature of 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0079] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0080] S1: Under argon protection, 20.65 g of 4,4-difluorobenzophenone, 46 g of 4A molecular sieve, 12.8 mL of aniline, and 74 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0081] S2: Add 24g of o-cresolphthalein, 12.1g of monomer, 14.8g of potassium carbonate, 72mL of toluene and 210mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0082] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0083] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0084] Step 2: Add 13.5g of flame retardant composite and 13.5g of corrosion resistant agent to 210mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash to obtain a corrosion-resistant flame retardant cloth.

[0085] Example 7: This example discloses a method for preparing a flame retardant composite, comprising the following steps:

[0086] Q1: 1.98 g of octamethylcyclotetrasiloxane and 1.32 g of γ-aminopropylmethyldimethoxysilane were added to a container, heated to 85°C and stirred, and then 0.12 g of potassium hydroxide was added. The temperature was then continued to rise to 100°C and the reaction was continued for 8 h. Then, 1.07 g of hexamethyldisiloxane was added and the reaction was continued for 1 h. After the reaction was completed, the mixture was rotary evaporated and the pH was adjusted to neutral to obtain compound 1;

[0087] Q2: Add 135.28g of diphenyl chlorophosphate to a container, then add 820mL of tetrahydrofuran, stir to dissolve, then mix 220.58g of compound 1 and 56.68g of triethylamine and place in a funnel. Add dropwise to the container at a low temperature of 3°C, control the addition time to be 4h, and after the addition is completed, heat to room temperature and react for 12h. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

[0088] This embodiment discloses a method for preparing a corrosion resistant agent, comprising the following steps:

[0089] S1: Under argon protection, 22.12 g of 4,4-difluorobenzophenone, 54 g of 4A molecular sieve, 13.6 mL of aniline, and 88 mL of toluene were added to a container. The temperature was raised to 160° C. and stirred for 24 h. After the reaction, the mixture was cooled, filtered, rotary evaporated, added to methanol for recrystallization, and dried at 70° C. for 12 h to obtain a monomer.

[0090] S2: Add 28g of o-cresolphthalein, 13.4g of monomer, 17.8g of potassium carbonate, 74.2mL of toluene and 231mL of N-methylpyrrolidone into a container, introduce nitrogen, heat at 150℃ with stirring and reflux for 1.5h, discharge the toluene in the water separator in batches, raise the temperature to 180℃ and react for 4h. After the reaction is completed, precipitate, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

[0091] This embodiment discloses a method for preparing a corrosion-resistant flame-retardant cloth, comprising the following steps:

[0092] Step 1: treating the aramid fiber cloth with a 0.5 mol / L sodium hydroxide solution to obtain pretreated aramid fiber;

[0093] Step 2: Add 22.8g of flame retardant composite and 16.2g of corrosion resistant agent to 205mL of phenolic epoxy resin containing 2g of light curing agent, ultrasonically stir for 12min to obtain an impregnation solution, add the pretreated aramid fiber to the impregnation solution and soak for 25min, cure, heat treat, and wash with water to obtain a corrosion-resistant flame retardant cloth.

[0094] Comparative Example 1: Compared with Example 1, in the process of preparing the corrosion-resistant flame-retardant cloth in Comparative Example 1, no flame retardant composite agent is added, and other conditions remain unchanged.

[0095] Comparative Example 2: Compared with Example 1, in Comparative Example 2, during the process of preparing the corrosion-resistant flame-retardant cloth, no corrosion-resistant agent was added, and other conditions remained unchanged.

[0096] The corrosion-resistant flame-retardant fabrics prepared in Examples 1-7 and Comparative Examples 1-2 were subjected to performance tests. The flame retardant properties of the samples were tested in accordance with GB / T17591-2006. Samples with an area of 20 cm*20 cm were immersed in an acidic environment with a relative humidity of 50% and a pH of 3.5 and an alkaline environment with a pH of 9.5 for 48 hours, respectively. The corrosion rate of the sample was calculated as: corrosion area / total area×100%. The test results are shown in Table 1.

[0097] Table 1

[0098]

[0099] The test results in Table 1 show that the flame retardant properties and corrosion resistance of flame-retardant fabrics can be effectively improved by using the methods of Examples 1-7. A comparison of Comparative Example 1 with Examples 1-7 shows that the addition of a flame retardant composite can effectively improve the flame retardant properties and corrosion resistance of the flame-retardant fabric; a comparison of Comparative Example 2 with Examples 1-7 shows that the addition of a corrosion inhibitor can effectively improve the corrosion resistance of the flame-retardant fabric.

[0100] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

[0101] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A method for preparing a corrosion-resistant flame-retardant cloth, characterized in that: The following steps are involved: Step 1: treating the aramid fiber cloth with alkali to obtain pretreated aramid fiber; Step 2: adding the flame retardant composite and the corrosion resistant agent to the phenolic epoxy resin containing the light curing agent, ultrasonically stirring to obtain an impregnation solution, adding the pretreated aramid fiber to the impregnation solution for immersion, curing, heat treatment, and water washing to obtain a corrosion-resistant flame retardant cloth.

2. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 1, characterized in that: In the step 1, a 0.5 mol / L sodium hydroxide solution is used for the alkali treatment process. In the step 2, the amount ratio of the flame retardant composite agent, the corrosion resistance agent and the phenolic epoxy resin is (12-25) g: (11-18) g: (150-220) mL.

3. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 1, characterized in that: The preparation method of the flame retardant composite comprises the following steps: Q1: Octamethylcyclotetrasiloxane and γ-aminopropylmethyldimethoxysilane were added to a container, heated and stirred to mix, potassium hydroxide was added, and the temperature was continued to react, and then hexamethyldisiloxane was added to continue the reaction. After the reaction was completed, rotary evaporation was performed and the pH was adjusted to neutral to obtain compound 1; Q2: Add diphenyl chlorophosphate to a container, then add tetrahydrofuran, stir to dissolve, then mix compound 1 with triethylamine and place in a funnel, add dropwise to the container under low temperature environment, control the addition time, and after the addition is completed, heat to room temperature for reaction. After the reaction is completed, filter, rotary evaporate, and vacuum dry to obtain a flame retardant composite.

4. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 3, characterized in that: In the Q1, the usage ratio of octamethylcyclotetrasiloxane, γ-aminopropylmethyldimethoxysilane, potassium hydroxide and hexamethyldisiloxane is (1.68-2.01) g: (1.01-1.35) g: (0.1-0.15) g: (0.88-1.14) g.

5. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 3, characterized in that: In the Q2, the usage ratio of diphenyl chlorophosphate, tetrahydrofuran, compound 1 and triethylamine is (123.45-143.52) g: (700-900) mL: (213.23-222.57) g: (52.11-59.83) g.

6. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 1, characterized in that: The preparation method of the corrosion resistant agent comprises the following steps: S1: Under argon protection, 4,4-difluorobenzophenone, 4A molecular sieve, aniline and toluene are added to a container, and the temperature is increased during mechanical stirring. The temperature is increased and stirred for reaction. After the reaction is completed, the mixture is cooled, filtered, rotary evaporated, recrystallized, and dried to obtain a monomer; S2: Add o-cresolphthalein, monomer, potassium carbonate, toluene and N-methylpyrrolidone into a container, introduce nitrogen, heat with stirring and reflux, discharge the toluene in the water separator in batches, raise the temperature to react, precipitate after the reaction, filter, vacuum dry, dissolve, precipitate, filter, wash, and vacuum dry to obtain a corrosion-resistant agent.

7. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 6, characterized in that: In the S1, the usage ratio of 4,4-difluorobenzophenone, 4A molecular sieve, aniline and toluene is (20.02-22.64) g: (45-55) g: (12.2-14.6) mL: (70-90) mL.

8. The method for preparing a corrosion-resistant flame-retardant cloth according to claim 6, characterized in that: In the S2, the usage ratio of o-cresolphthalein, monomer, potassium carbonate, toluene and N-methylpyrrolidone is (20-30) g: (11-13.5) g: (14.2-18.4) g: (70-75) mL: (200-234) mL.

9. The corrosion-resistant flame-retardant cloth prepared by the preparation method according to any one of claims 1 to 8.

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