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CN-122011980-A - Corrosion-resistant flame-retardant fireproof sealant material and preparation method thereof

CN122011980ACN 122011980 ACN122011980 ACN 122011980ACN-122011980-A

Abstract

The invention discloses a corrosion-resistant flame-retardant fireproof sealant material and a preparation method thereof, belongs to the technical field of sealant preparation, and is used for solving the technical problems that in the prior art, the sealant is resistant to organic liquid corrosion and the flame retardant performance is to be further improved; according to the invention, the phosphazene-silicon epoxy flame-retardant phase, the catechol phosphonic acid bonding phase and the boron-nitrogen coordination hole sealing phase are cooperatively introduced into the sealant system, and a continuous and stable multiphase network structure is constructed through a stepwise reaction and a curing process, so that the flame retardance, anti-adhesion enhancement and pore regulation effects of the sealant are remarkably improved, the obtained sealant meets the flame retardance and fireproof performance requirements, and meanwhile, has good flexibility and structural integrity, and experimental results show that the sealant has higher retention rate of mechanical performance after the effect of a liquid medium, and shows excellent corrosion resistance and environmental adaptability.

Inventors

  • LIU ZHITONG
  • LIU HEPING

Assignees

  • 汇泰消防科技河北有限公司

Dates

Publication Date
20260512
Application Date
20260211

Claims (10)

  1. 1. The corrosion-resistant flame-retardant fireproof sealant material is characterized by comprising the following raw materials, by weight, 40-50 parts of phosphazene silicon epoxy flame-retardant phase, 30-40 parts of catechol phosphonic acid bonding phase, 18-21 parts of boron-nitrogen coordination hole sealing phase, 6-8 parts of dioctyl phthalate and 4-6 parts of fumed silica; the preparation method of the phosphazene silicon epoxy flame retardant phase comprises the following steps: A1, adding an allylsilane phosphazene intermediate and tetrahydrofuran into a reaction kettle, stirring until the materials are uniformly dispersed, adding deionized water and glacial acetic acid, heating the reaction kettle to 40-50 ℃, stirring for 3-5 hours at a constant temperature, and distilling under reduced pressure until no liquid is extracted after the reaction is finished to obtain a phosphazene silica flame retardant intermediate; a2, adding the phosphazene silicon oxide flame-retardant intermediate and tetrahydrofuran into a reaction kettle, stirring until the mixture is uniformly dispersed, adding an oxidant, adding 98wt% of concentrated sulfuric acid, controlling the temperature of the reaction kettle to be 50-60 ℃, keeping the temperature, stirring for 4-6 hours, and performing post treatment to obtain the phosphazene silicon oxide flame-retardant phase.
  2. 2. The corrosion-resistant flame-retardant and fireproof sealant material according to claim 1, wherein in the step A1, the usage ratio of allylsilane phosphazene intermediate, tetrahydrofuran, deionized water and glacial acetic acid is 18-20 g/100 mL/30-40 mL/1-2 mL.
  3. 3. The corrosion-resistant flame-retardant and fireproof sealant material according to claim 1, wherein in the step A2, the phosphazene silica flame-retardant intermediate, tetrahydrofuran, oxidant and 98wt% concentrated sulfuric acid are used in an amount ratio of 15-18g to 80mL to 18-21mL to 0.4-0.6mL, and the oxidant is 30wt% hydrogen peroxide aqueous solution.
  4. 4. The corrosion-resistant flame-retardant fireproof sealant material according to claim 1, wherein the preparation method of the allylsilane phosphazene intermediate comprises the steps of adding hexachlorocyclotriphosphazene and tetrahydrofuran into a reaction kettle, stirring until the hexachlorocyclotriphosphazene and tetrahydrofuran are dissolved, introducing nitrogen for protection, cooling the reaction kettle to 0-5 ℃, adding p-allylphenol, 3-aminopropyl triethoxysilane and triethylamine, heating the reaction kettle to 35-45 ℃ after stirring for 40-60min, stirring for 5-7h after heating, filtering for desalting after the reaction is finished, and distilling the solution under reduced pressure until no liquid is produced, thus obtaining the allylsilane phosphazene intermediate.
  5. 5. The corrosion-resistant flame-retardant and fireproof sealant material according to claim 4, wherein the dosage ratio of hexachlorocyclotriphosphazene, tetrahydrofuran, p-allylphenol, 3-aminopropyl triethoxysilane and triethylamine is 9-12 g/100 mL/6-8 g/8-10 mL/10 mL.
  6. 6. The corrosion-resistant flame-retardant and fire-retardant sealant material according to claim 1, wherein the catechol phosphonic acid binding phase is prepared by the following method: B1, adding catechol and methylene dichloride into a reaction kettle, stirring until the catechol and the methylene dichloride are dissolved, cooling the reaction kettle to 0-5 ℃ under the protection of nitrogen, adding triethylamine, adding the acryloyl chloride in ten batches at equal intervals for 5-8min, heating the reaction kettle to 20-25 ℃ after the addition is finished, carrying out heat preservation and stirring for 3-5h, filtering to remove salt after the reaction is finished, carrying out reduced pressure distillation until no liquid is extracted, and preserving the reaction kettle in a dark place to obtain an acrylic ester catechol monomer; And B2, adding the acrylic ester catechol monomer and N, N-dimethylformamide into a reaction kettle, stirring, adding vinyl phosphonic acid and azodiisobutyronitrile after the acrylic ester catechol monomer and N, N-dimethylformamide are uniformly dispersed, introducing nitrogen for protection, heating the reaction kettle to 60-70 ℃, preserving heat, stirring for 6-8h, and performing post treatment to obtain catechol phosphonic acid bonding phase.
  7. 7. The corrosion-resistant flame-retardant fireproof sealant material according to claim 6, wherein in the step B1, the dosage ratio of catechol, dichloromethane, triethylamine and acryloyl chloride is 10-12 g/100 mL/10-12 mL/8-10 mL, and in the step B2, the dosage ratio of the enoate catechol monomer, N-dimethylformamide, vinylphosphonic acid and azodiisobutyronitrile is 12-16 g/100 mL/8-10 g/1 g.
  8. 8. The corrosion-resistant flame-retardant fireproof sealant material according to claim 1, wherein the preparation method of the boron-nitrogen coordination hole sealing phase is characterized in that boric acid, triethanolamine and 1, 2-propylene glycol are added into a reaction kettle, stirred until the mixture is uniform, the reaction kettle is heated to 110-120 ℃, then 2-methylimidazole is added, the temperature is continuously raised to 120-130 ℃, the heat preservation reaction is carried out for 2-4 hours, and the boron-nitrogen coordination hole sealing phase is obtained after post treatment.
  9. 9. The corrosion-resistant flame-retardant fireproof sealant material according to claim 8, wherein in the process of preparing the boron-nitrogen coordination hole sealing phase, the dosage ratio of boric acid, triethanolamine, 1, 2-propanediol and 2-methylimidazole is 8-10g:10-12mL:4-6mL:0.6-0.8g.
  10. 10. The method for preparing the corrosion-resistant flame-retardant fireproof sealant material according to any one of claims 1 to 9, which is characterized by comprising the steps of adding a phosphazene silicon epoxy flame-retardant phase, a catechol phosphonic acid bonding phase and a boron-nitrogen coordination hole sealing phase into a vacuum stirring kettle, heating the vacuum stirring kettle to 25-35 ℃, carrying out heat preservation and stirring for 20-40min, then adding dioctyl phthalate, continuing stirring for 15-25min, adding fumed silica, stirring until dry powder agglomeration is even, and then carrying out vacuum defoaming to obtain the sealant material.

Description

Corrosion-resistant flame-retardant fireproof sealant material and preparation method thereof Technical Field The invention relates to the technical field of sealant preparation, in particular to a corrosion-resistant flame-retardant fireproof sealant material and a preparation method thereof. Background Along with the continuous improvement of the performance requirements of sealing materials in the fields of construction, transportation and industry, the flame-retardant fireproof sealing adhesive material gradually becomes one of key technologies, the sealing adhesive is required to meet the basic requirements of flame retardance and fireproof performance, has good corrosion resistance, can maintain the mechanical performance and structural integrity of the sealing adhesive material after being exposed to various chemical media and humid environments for a long time, is currently common in the market and depends on an organic polymer matrix, and combines different flame-retardant fillers or auxiliary agents, such as inorganic flame retardants, phosphorus flame-retardant materials and the like, so that the flame-retardant effect is achieved, however, when the materials face complex environmental conditions, the problems of insufficient corrosion resistance, aging acceleration and the like are often faced, and the long-term service performance of the materials is difficult to ensure. Although the existing flame-retardant fireproof sealant materials have a certain progress in flame-retardant performance, the prior flame-retardant fireproof sealant materials still have great defects in corrosion resistance, durability and structural stability, most of traditional materials depend on single flame-retardant fillers or reinforcing components, so that the problems of mechanical property attenuation, interface mismatch and the like are easy to occur in complex environments, particularly in organic media or liquid corrosion environments, the defects not only influence the long-term service performance of the materials, but also cause instability in the bearing and extending processes, and the requirements of corrosion resistance, ageing resistance and flame retardance fireproof multiple performances in high-requirement application scenes are difficult to meet. In addition, in the prior art, the flame retardance and the corrosion resistance are usually realized through simple physical mixing, but the depth regulation and control are not carried out on the molecular structure level, so that the molecular structure of the material often fails to form effective synergistic action, the performance of the material under the conditions of thermal action, liquid medium or high temperature is further influenced, especially at high temperature, the thermal stability and the combustion evolution path of the prior material are difficult to effectively control, the structure of the material is easy to damage, and a stable thermal response mechanism is not available, so that the consistent performance cannot be maintained in complex application. Disclosure of Invention The invention aims to provide a corrosion-resistant flame-retardant fireproof sealant material and a preparation method thereof, which are used for solving the technical problems that in the prior art, the sealant is resistant to organic liquid corrosion and the flame retardant performance is to be further improved. The aim of the invention can be achieved by the following technical scheme: the corrosion-resistant flame-retardant fireproof sealant material comprises the following raw materials, by weight, 40-50 parts of phosphazene silicon epoxy flame-retardant phase, 30-40 parts of catechol phosphonic acid bonding phase, 18-21 parts of boron-nitrogen coordination hole sealing phase, 6-8 parts of dioctyl phthalate and 4-6 parts of fumed silica; Further, the preparation method of the phosphazene silicon epoxy flame retardant phase comprises the following steps: A1, adding an allylsilane phosphazene intermediate and tetrahydrofuran into a reaction kettle, stirring until the materials are uniformly dispersed, adding deionized water and glacial acetic acid, heating the reaction kettle to 40-50 ℃, stirring for 3-5 hours at a constant temperature, and distilling under reduced pressure until no liquid is extracted after the reaction is finished to obtain a phosphazene silica flame retardant intermediate; a2, adding the phosphazene silicon oxide flame-retardant intermediate and tetrahydrofuran into a reaction kettle, stirring until the mixture is uniformly dispersed, adding an oxidant, adding 98wt% of concentrated sulfuric acid, controlling the temperature of the reaction kettle to be 50-60 ℃, keeping the temperature, stirring for 4-6 hours, and performing post treatment to obtain the phosphazene silicon oxide flame-retardant phase. The reaction principle for preparing the phosphazene silicon epoxy flame retardant phase is as follows: The alkoxysilane structure in the all