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CN-121991261-A - Biomass flame retardant and preparation method and application thereof

CN121991261ACN 121991261 ACN121991261 ACN 121991261ACN-121991261-A

Abstract

The invention provides a biomass flame retardant, a preparation method and application thereof, and belongs to the technical field of flame retardants. The preparation method comprises the steps of adding sodium alginate and phosphoric acid into a solvent, heating and reacting at 95-100 ℃ under stirring to obtain a solution A, cooling the solution A to 40-60 ℃ and regulating the pH value to 6-7, adding urea, continuously reacting at 70-80 ℃ to obtain a solution B, centrifuging, washing and drying the solution B to obtain the biomass flame retardant (SAPU). The invention adopts water as solvent, reduces the production cost, is environment-friendly, does not need to add other flame retardants, and has good flame retardance when the adding amount of SAPU reaches 16 wt percent, the T 1 and the t 2 of the flame-retardant epoxy resin are both 1s, the LOI value reaches 31.3 percent, and the UL-94 is V-0 grade.

Inventors

  • ZHANG XIAOQIAN
  • LIU SONG
  • LI JI
  • QIU PING
  • ZHAO RUOHAN
  • CHAO CHUNYAN
  • ZHANG JUNSONG
  • GAO MING

Assignees

  • 华北科技学院(中国煤矿安全技术培训中心)

Dates

Publication Date
20260508
Application Date
20260122

Claims (10)

  1. 1. The preparation method of the biomass flame retardant is characterized by comprising the following steps: (1) Adding sodium alginate and phosphoric acid into water, and heating and reacting at 95-100 ℃ under stirring to obtain a solution A; (2) Cooling the solution A to 40-60 ℃, regulating the pH to 6-7, adding urea, and continuing to react at 70-80 ℃ to obtain a solution B; (3) And centrifuging, washing and drying the solution B to obtain the biomass flame retardant.
  2. 2. The preparation method of the biomass flame retardant according to claim 1, wherein in the step (1), the amount of sodium alginate is 4-5 g, the amount of phosphoric acid aqueous solution with the mass concentration of 85% is 13-14 mL, and in the step (2), the amount of urea is 3-4 g.
  3. 3. The preparation method of the biomass flame retardant according to claim 2, wherein in the step (1), the amount of sodium alginate is 4.5 g, the amount of phosphoric acid aqueous solution with the mass concentration of 85% is 13.5 mL, and in the step (2), the amount of urea is 3.6 g.
  4. 4. A process for preparing a biomass flame retardant according to any of claims 1 to 3, wherein in step (1), the reaction time is 1 to 2 h.
  5. 5. The method for preparing a biomass fire retardant according to claim 1, wherein in the step (2), ammonia water is added dropwise to adjust the pH to 6-7.
  6. 6. The method for preparing a biomass fire retardant according to claim 1, wherein in the step (2), the reaction is carried out at 70-80 ℃ for 1-1.5 h.
  7. 7. A biomass flame retardant prepared by the preparation method of any one of claims 1-6.
  8. 8. Use of the biomass flame retardant according to claim 7 for the preparation of flame retardant epoxy resins.
  9. 9. The method according to claim 8, wherein the flame-retardant epoxy resin is prepared from the following raw materials, by mass, 42-46 wt% of epoxy resin E-44, 42-46 wt% of curing agent PA650 and 8-16 wt% of biomass flame retardant.
  10. 10. The method according to claim 9, wherein the flame-retardant epoxy resin is prepared from the following raw materials, by mass, 42 wt% of epoxy resin E-44, 42 wt% of curing agent PA650 and 16 wt% of biomass flame retardant.

Description

Biomass flame retardant and preparation method and application thereof Technical Field The invention relates to the technical field of flame retardants, in particular to a biomass flame retardant and a preparation method and application thereof. Background In the prior literature, few studies on modification of alginate by phosphorus/nitrogen for flame retardant polymers have been reported. Although other biomass flame retardant modifications are reported, most of the biomass flame retardant modifications adopt organic solvents, so that the biomass flame retardant is easy to remain in environment pollution. For example, the organic solvents N, N-dimethylformamide and the like are expensive on the one hand and troublesome in the subsequent separation of the flame retardant product on the other hand, require multiple washing to remove the organic solvents, and increase the production process and cost. The UL-94 rating V-0 standard is that at least 5 samples per group, no sample burn for more than 10 seconds after the test flame is removed, no sample burn up to the clamp, no sample burn melt drop down to ignite the underlying cotton, and no sample at the same time, after the test flame is removed for a second time, a reddish burn is continued for more than 30 seconds. The existing biomass flame retardant is still faced with the problems of complex preparation method, large addition amount and low flame retardant efficiency when being used for preparing flame retardant epoxy resin. For example, although there are also those which reach the UL-94 level V-0, the duration t 2 of the second ignition is still longer and needs to be further improved. Therefore, there is a need for further development of bio-based flame retardants that are efficient, inexpensive and easy to prepare. Disclosure of Invention The biomass flame retardant and the preparation method and application thereof provided by the invention adopt water as a solvent, reduce the production cost, are environment-friendly, do not need to add other flame retardants, and have very good flame retardance when the adding amount of SAPU reaches 16 wt%, the T 1 and the t 2 of the flame-retardant epoxy resin are both 1 s, the LOI value reaches 31.3%, and the UL-94 is V-0 level. The technical scheme of the invention is realized in that the preparation method of the biomass flame retardant comprises the following steps: (1) Adding Sodium Alginate (SA) and phosphoric acid into a solvent, and heating and reacting at 95-100 ℃ under the condition of stirring to obtain a solution A; (2) Cooling the solution A to 40-60 ℃, regulating the pH to 6-7, adding urea, and continuing to react at 70-80 ℃ to obtain a solution B; (3) And centrifuging, washing and drying the solution B to obtain the biomass flame retardant (SAPU). The synthetic route of the biomass flame retardant is as follows: Further, in the step (1), the dosage of sodium alginate is 4-5 g, the dosage of phosphoric acid aqueous solution with the mass concentration of 85% is 13-14 mL, and in the step (2), the dosage of urea is 3-4 g. Further, in the step (1), the amount of sodium alginate is 4.5g, the amount of phosphoric acid aqueous solution with the mass concentration of 85% is 13.5 mL, and in the step (2), the amount of urea is 3.6 g. Further, in the step (1), the reaction time is 1 to 2 h. Further, in the step (2), ammonia water is added dropwise to adjust the pH to 6-7. Further, in the step (2), 1 to 1.5 h is reacted at 70 to 80 ℃. A biomass flame retardant is prepared by the preparation method. Use of a biomass flame retardant in the preparation of flame retardant epoxy resins (EP). Further, the flame-retardant epoxy resin is prepared from the following raw materials, by mass, 42-46-wt% of epoxy resin E-44, 42-46-wt% of curing agent PA650 and 8-16-wt% of biomass flame retardant. Further, the flame-retardant epoxy resin is prepared from the following raw materials, by mass, 42 wt% of epoxy resin E-44, 42 wt% of curing agent PA650 and 16 wt% of biomass flame retardant. The invention has the beneficial effects that: according to the preparation of the biomass flame retardant, water is used as a solvent, and the marine extract alginate with abundant resources is reacted with the urea and the phosphoric acid with low price, so that the production cost is reduced, the preparation process is easy and convenient, and compared with the use of an organic solvent, the biomass flame retardant is environment-friendly. When the flame-retardant epoxy resin is prepared, other flame retardants are not required to be added, and only the SAPU provided by the invention is required to be added. The SAPU prepared by the invention is added into EP, and the densification and graphitization of the carbon layer are realized by catalytic dehydration and promotion of carbon skeleton rearrangement in a condensed phase during combustion, so that the carbon layer is continuous and dense without holes and cracks, thereby enhancing the th