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CN-121991132-A - Phosphorus-nitrogen-boron synergistic smoke suppression flame retardant and preparation method thereof

CN121991132ACN 121991132 ACN121991132 ACN 121991132ACN-121991132-A

Abstract

The invention belongs to the field of functional finishing of textiles, and particularly relates to a phosphorus-nitrogen-boron synergistic smoke suppression flame retardant and a preparation method thereof. When the flame retardant is prepared, cyanuric chloride, phosphoric acid and a solvent are added into a reaction device, heated and stirred, ammonia water is used for regulating pH until the reaction is completed, then reduced pressure distillation is carried out, and the intermediate product 1 is obtained after purification and drying. Boric acid, mannitol and solvent are added into a reaction bottle, heated and stirred, and after the reaction is finished, the intermediate product 2 is obtained by distillation and drying. And adding the intermediates 1 and 2 into a reaction bottle containing a solvent, heating and stirring, adjusting the pH value by ammonia water, and distilling, purifying and drying after the reaction is finished to obtain the target flame retardant. The flame retardant contains three flame retardant elements of phosphorus, nitrogen and boron, which can play a role in synergistic flame retardance, so that the synthesized target flame retardant has an excellent flame retardance effect.

Inventors

  • DONG CHAOHONG
  • LV ZHOU
  • ZHAO LIXING
  • ZHANG TIAN
  • WANG JIALE
  • ZHAO WENQI

Assignees

  • 青岛大学

Dates

Publication Date
20260508
Application Date
20260121

Claims (8)

  1. 1. The phosphorus-nitrogen-boron durable flame retardant is characterized by comprising the following chemical structure: 。
  2. 2. The method for preparing the phosphorus-nitrogen-boron durable flame retardant according to claim 1, wherein the synthesis steps are as follows: (1) Adding phosphoric acid and cyanuric chloride with a certain molar ratio and a solvent into a reaction device, heating to 70-110 ℃, stirring until the mixture is dissolved, adjusting pH to be 6-7 by ammonia water, reacting for 9-12 h, performing reduced pressure distillation to remove the solvent, washing, purifying and drying to obtain an intermediate product 1; (2) Adding boric acid and mannitol with a certain molar ratio and a solvent into a reaction device, stirring until the boric acid and mannitol are dissolved, heating to 90-110 ℃, reacting for 9-12 h, and distilling and drying to obtain an intermediate product 2 after the reaction is finished; (3) And adding the intermediate 1, the intermediate 2 and the solvent into a reaction device, heating to 110-120 ℃ for continuous reaction for 5-8 hours, adjusting pH to be 6-7 by ammonia water, performing reduced pressure distillation after the reaction is finished, and drying to constant weight to obtain the target flame retardant.
  3. 3. The method for preparing a phosphorus-nitrogen-boron durable flame retardant according to claim 2, wherein the molar ratio of phosphoric acid to cyanuric chloride in the step (1) is 2:1.
  4. 4. The method for preparing a phosphorus-nitrogen-boron durable flame retardant according to claim 2, wherein the solvent in the step (1) is any one of toluene, acetonitrile, tetrahydrofuran, dichloromethane and 1, 4-dioxane or a mixture thereof in any proportion.
  5. 5. The method for preparing a durable flame retardant according to claim 2, wherein the molar ratio of boric acid to mannitol in the step (2) is 3:1.
  6. 6. The method for preparing a durable flame retardant according to claim 2, wherein the solvent in the step (2) is any one of water, toluene, ethanol, methanol, methylene chloride and N, N-dimethylformamide or a mixture thereof in any proportion.
  7. 7. The method for preparing a phosphorus-nitrogen-boron durable flame retardant according to claim 2, wherein the molar ratio of the intermediate product 1 to the intermediate product 2 in the step (3) is 3:1.
  8. 8. The method for preparing a durable flame retardant according to claim 2, wherein the solvent in the step (3) is any one of water, ethanol, acetonitrile, methylene chloride and N, N-dimethylformamide or a mixture thereof in any proportion.

Description

Phosphorus-nitrogen-boron synergistic smoke suppression flame retardant and preparation method thereof Technical Field The invention belongs to the field of functional finishing of textiles, and particularly relates to a phosphorus-nitrogen-boron durable flame retardant and a preparation method thereof. Background Cotton fabrics are widely selected by people during shopping because of their good softness, comfort and other characteristics. However, since the limit oxygen index of cotton fabrics is low, they are easy to burn when they meet fire sources, which may cause fire accidents to occur, resulting in casualties and property loss. With the increasing demands on material safety and environmental friendliness, research and development of synthetic flame retardants is becoming increasingly important. Currently, researchers have synthesized various series of flame retardants, for example, halogen-based, nitrogen-based, phosphorus-based, silicon-based, and the like. However, halogen flame retardants (such as brominated and chlorinated flame retardants) have been used in many countries and regions to limit and prohibit the use of halogen flame retardants because they release toxic hydrogen halide gases and persistent organic pollutants during combustion, which are potentially dangerous to the environment and human health. A single phosphorus-containing flame retardant often does not achieve an excellent flame retardant effect, and in recent years, a great deal of research has focused on improving flame retardant efficiency by synergistic action of phosphorus with other environmentally friendly flame retardant elements such as nitrogen, silicon, and boron. The conventional flame retardant mainly contains phosphorus and nitrogen, and the phosphorus-nitrogen flame retardant has obvious effect in the field of cotton fabric flame retardance, but the flame retardant has the defect of releasing a large amount of smoke in the process of playing a flame retardance role, and has not been solved effectively. In order to solve the problem of large smoke content released by the conventional phosphorus-containing flame retardant, the conventional cotton flame retardant is prepared by adding metal ions, organic silicon, organic boron and the like into a system. Although the metal-based flame retardant can effectively reduce heat release and smoke emission, the application of the metal-based flame retardant in cotton fabrics is often limited by fabric hardening, color change and metal ion environmental problems. Silicon-based flame retardants reduce smoke emissions by promoting the formation of a dense char layer, but tend to sacrifice fabric softness, breathability, and wear comfort, limiting their practical application in cotton textiles. Among the commonly used low smoke flame retardants, boron-based flame retardants are approved for their excellent properties. The flame retardant is popular in terms of high efficiency, and the smoke and toxic substances generated during combustion are very little, so that the flame retardant completely meets the requirements of the current market on environment-friendly, efficient and energy-saving solutions According to the invention, three elements of phosphorus, nitrogen and boron are synergistically proportioned, and through the synergistic effect of the boron element on the phosphorus-nitrogen flame-retardant system, the flame-retardant efficiency is ensured, the smoke release is obviously reduced, and the char formation and various physical properties are excellent. The flame retardant has a plurality of reactive groups, and can form stable covalent bonding with cotton fibers, so that the flame retardant performance is still reliable after multiple water washes. The fabric can obtain flame retardant function through a conventional after-finishing mode, so that the process flow is shortened, the cost and the energy consumption are reduced, and no toxic byproducts are generated. The flame retardant has the advantages of no harmful formaldehyde release in the use process, less smoke content generated during combustion, good flame retardant property and thermal stability, and not only ensuring the health and safety of users, but also reducing the environmental load. The flame retardant can be subjected to industrialized research in the later period, and has good application value and social benefit. Disclosure of Invention The invention aims to solve the technical problem of providing a phosphorus-nitrogen-boron durable flame retardant and a preparation method thereof, wherein groups containing phosphorus elements and nitrogen elements are respectively grafted on the basis of a boron-containing structure, and the synthesized flame retardant has high-efficiency flame retardant performance, is green and pollution-free, and has high product purity. The technical scheme adopted is as follows: A phosphorus nitrogen boron durable flame retardant, the chemical structure of which is as follows