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CN-122011500-A - Flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, and preparation method and application thereof

CN122011500ACN 122011500 ACN122011500 ACN 122011500ACN-122011500-A

Abstract

The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, a preparation method and application thereof, wherein the preparation method comprises the steps of preparing DMSO intercalated kaolin, preparing potassium acetate intercalated kaolin, preparing phenylphosphonic acid intercalated kaolin, adding the phenylphosphonic acid intercalated kaolin into chitosan aqueous solution, immersing the phenylphosphonic acid intercalated kaolin into the polyurethane foam, continuously stirring slowly, taking out and drying after immersing, soaking in glutaraldehyde ethanol solution, stirring, taking out and drying to obtain the flame-retardant polyurethane soft foam. According to the invention, the chitosan-coated phenylphosphonic acid intercalated kaolin coating prepared by the steps has low heat release rate and smoke release rate, and has excellent flame retardant property, and the chitosan-coated phenylphosphonic acid intercalated kaolin coating and the flame retardant polyurethane soft foam can obviously reduce the release rate and smoke generation rate of combustible gas under the condition of heat exposure.

Inventors

  • MIAO YANG
  • Zhai Qianhe
  • LUO YI
  • WU YAOPENG
  • LI YUNXIA
  • MA CHAO

Assignees

  • 太原理工大学
  • 山西金宇科林科技有限公司

Dates

Publication Date
20260512
Application Date
20260309

Claims (10)

  1. 1. A preparation method of flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin is characterized by comprising the following steps: s1, adding kaolin powder into dimethyl sulfoxide and water, performing intercalation treatment under magnetic stirring, and centrifugally drying to obtain DMSO intercalated kaolin; s2, adding the DMSO intercalated kaolin obtained in the S1 into a potassium acetate aqueous solution, performing replacement intercalation treatment under magnetic stirring, and centrifugally drying to obtain potassium acetate intercalated kaolin; s3, adding the potassium acetate intercalated kaolin in the S2 into a phenylphosphonic acid aqueous solution, performing replacement intercalation treatment under magnetic stirring, and centrifugally drying to obtain the phenylphosphonic acid intercalated kaolin; S4, adding the phenylphosphonic acid intercalated kaolin obtained in the step S3 into a chitosan aqueous solution, mixing under magnetic stirring, immersing into polyurethane foam, continuously slowly stirring, taking out and drying after immersing, and obtaining an intermediate polyurethane foam; And S5, soaking the intermediate polyurethane foam in the step S4 in glutaraldehyde ethanol solution, stirring, taking out and drying to obtain the flame-retardant polyurethane soft foam.
  2. 2. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is characterized in that in S1, the mass ratio of kaolin powder to dimethyl sulfoxide to water is 1:7:2, the temperature of magnetic stirring is 50-60 ℃, the time of magnetic stirring is 12-36h, and methanol is added for cleaning during centrifugation.
  3. 3. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is characterized in that in S2, the mass ratio of DMSO intercalated kaolin to potassium acetate to water is 3:40:16, the temperature of magnetic stirring is 20-25 ℃, the rotating speed of magnetic stirring is 400-600r/min, the time of magnetic stirring is 12-36h, and absolute ethyl alcohol is added for cleaning during centrifugation.
  4. 4. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is characterized in that in S3, the mass ratio of potassium acetate intercalated kaolin to phenylphosphonic acid to water is 1:5:20, the temperature of magnetic stirring is 20-25 ℃, the time of magnetic stirring is 12-36h, the rotating speed of magnetic stirring is 400-600r/min, and absolute ethyl alcohol is added for cleaning during centrifugation.
  5. 5. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin, which is disclosed in claim 1, is characterized in that in S4, the mass ratio of the phenylphosphonic acid intercalated kaolin to the chitosan to the water is 2:1:100, the temperature of magnetic stirring is 20-25 ℃, and the rotating speed of the magnetic stirring is 100-300r/min.
  6. 6. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is characterized in that in S4, the polyurethane foam is immersed and then vacuumized, the immersing temperature is 20-25 ℃, the rotating speed of slow stirring is 80-200r/min, and the time of slow stirring is 4-6h.
  7. 7. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin, according to claim 1, wherein in S5, the concentration of glutaraldehyde ethanol solution is 0.5-2mol/L, the stirring speed is 80-200r/min, and the stirring time is 1-3h.
  8. 8. The preparation method of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin, as claimed in claim 1, is characterized in that in S1-S5, the drying temperature is 50-100 ℃, and the drying time is 2-5h.
  9. 9. A flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin, which is characterized in that the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is prepared by the preparation method of any one of claims 1 to 8.
  10. 10. The application of the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is characterized in that the flame-retardant polyurethane soft foam based on the phenylphosphonic acid intercalated kaolin is applied to the preparation of high-temperature heat insulation and heat protection materials for building heat preservation, transportation and aerospace.

Description

Flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, and preparation method and application thereof Technical Field The invention relates to the technical field of flame-retardant materials, in particular to a flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, and a preparation method and application thereof. Background The coal-series kaolin is solid waste generated in the coal exploitation and washing process, and the main component is kaolin, and contains a small amount of coal and inorganic minerals. The carbon content is low, the heat value is not high, but the reserve is huge, the soil is occupied by long-term accumulation, and the pollution problem caused to the environment needs to be solved. In recent years, coal gangue is gradually recycled, and the coal gangue can be used for power generation, brick making, paving, backfilling mines, extracting useful minerals and the like. After the coal-series kaolin is calcined, the coal-series kaolin is added into the production processes of coating, papermaking and the like, so that the environmental pollution can be reduced, the economic value can be created, and the development of recycling economy can be promoted. The kaolin can be used as an important filler of the flame-retardant coating, and has multiple advantages of improving the comprehensive performance of the coating, being wide in source, low in cost and the like due to the physical barrier effect of the kaolin and being used as a general filler. The flame retardant can be used as a high-efficiency synergistic flame retardant to improve the system performance, can also meet the basic filler function of the coating, and plays an indispensable role in developing high-performance and environment-friendly flame retardant coatings. Modification (such as calcination, surface modification and intercalation) of kaolin can further improve the dispersibility and flame retardant efficiency of kaolin in the flame retardant coating. Disclosure of Invention The invention aims to provide a flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, a preparation method and application thereof, and the prepared chitosan-coated phenylphosphonic acid intercalated kaolin coating has low heat release rate and smoke release rate and excellent flame-retardant property. In order to achieve the above purpose, the invention provides a preparation method of flame-retardant polyurethane soft foam based on phenylphosphonic acid intercalated kaolin, which comprises the following steps: s1, adding kaolin powder into dimethyl sulfoxide and water, performing intercalation treatment under magnetic stirring, and centrifugally drying to obtain DMSO intercalated kaolin; s2, adding the DMSO intercalated kaolin obtained in the S1 into a potassium acetate aqueous solution, performing replacement intercalation treatment under magnetic stirring, and centrifugally drying to obtain potassium acetate intercalated kaolin; s3, adding the potassium acetate intercalated kaolin in the S2 into a phenylphosphonic acid aqueous solution, performing replacement intercalation treatment under magnetic stirring, and centrifugally drying to obtain the phenylphosphonic acid intercalated kaolin; S4, adding the phenylphosphonic acid intercalated kaolin obtained in the step S3 into a chitosan aqueous solution, mixing under magnetic stirring, immersing into polyurethane foam, continuously slowly stirring, taking out and drying after immersing, and obtaining an intermediate polyurethane foam; And S5, soaking the intermediate polyurethane foam in the step S4 in glutaraldehyde ethanol solution, stirring, taking out and drying to obtain the flame-retardant polyurethane soft foam. Preferably, in S1, the mass ratio of kaolin powder to dimethyl sulfoxide to water is 1:7:2, the temperature of magnetic stirring is 50-60 ℃, the time of magnetic stirring is 12-36h, and methanol is added for cleaning during centrifugation. Preferably, in S2, the mass ratio of DMSO intercalated kaolin, potassium acetate and water is 3:40:16, the temperature of magnetic stirring is 20-25 ℃, the rotating speed of magnetic stirring is 400-600r/min, the time of magnetic stirring is 12-36h, and absolute ethyl alcohol is added for cleaning during centrifugation. Preferably, in S3, the mass ratio of the potassium acetate intercalated kaolin to the phenylphosphonic acid to the water is 1:5:20, the temperature of magnetic stirring is 20-25 ℃, the time of magnetic stirring is 12-36h, the rotating speed of magnetic stirring is 400-600r/min, and absolute ethyl alcohol is added for cleaning during centrifugation. Preferably, in S4, the mass ratio of the phenylphosphonic acid intercalated kaolin to the chitosan to the water is 2:1:100, the temperature of the magnetic stirring is 20-25 ℃, and the rotating speed of the magnetic stirring is 100-300r/min. Preferably, in S4, the polyurethane foam is