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Phosphorus-nitrogen type flame retardant as well as preparation method and application thereof

A technology of flame retardant and phosphorus nitrogen, which is applied in the field of flame retardants, can solve the problems of not being resistant to washing, poor hand feeling, etc., and achieve the effects of small loss of strength, environmental protection and pollution-free application, and improved flame retardant efficiency

Active Publication Date: 2021-08-13
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the viscose fibers finished after flame retardant are not resistant to washing and have the disadvantages of poor hand feeling

Method used

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  • Phosphorus-nitrogen type flame retardant as well as preparation method and application thereof
  • Phosphorus-nitrogen type flame retardant as well as preparation method and application thereof
  • Phosphorus-nitrogen type flame retardant as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Synthesis of intermediate neopentyl glycol phosphorus oxychloride

[0036] Add 0.1mol of neopentyl glycol to a three-necked flask equipped with a spherical condenser, thermometer and magnetic stirring device, then add 50mL of dichloromethane as a solvent, stir to completely dissolve neopentyl glycol in the solvent, and keep the temperature at 3°C , and then add 0.11mol phosphorus oxychloride dropwise, after the dropwise addition, the temperature is raised to 55°C, and the reaction is continued for 5h until no hydrogen chloride is released; after the reaction is completed, cool to room temperature, and distill off the solvent and unreacted trichloride under reduced pressure Oxyphosphorus, washed three times with n-hexane, and vacuum-dried to obtain the intermediate neopentyl glycol phosphorus oxychloride.

[0037] 2. Preparation of phosphorus nitrogen flame retardant

[0038] Under the protection of nitrogen atmosphere, dissolve 0.05 mol of imidazole in 50 mL of dich...

Embodiment 2

[0047] 1. Synthesis of intermediate neopentyl glycol phosphorus oxychloride

[0048] Add 0.2mol of neopentyl glycol to a three-neck flask equipped with a spherical condenser, thermometer and magnetic stirring device, then add 100mL of dichloromethane as a solvent, stir to completely dissolve neopentyl glycol in the solvent, and keep the temperature at 3°C , then add 0.22mol phosphorus oxychloride dropwise, after the dropwise addition, the temperature is raised to 55°C, and the reaction is continued for 5h until no hydrogen chloride is released; after the reaction is completed, cool to room temperature, and distill off the solvent and unreacted trichloride under reduced pressure Oxyphosphorus, washed three times with n-hexane, and vacuum-dried to obtain the intermediate neopentyl glycol phosphorus oxychloride.

[0049] 2. Preparation of phosphorus nitrogen flame retardant

[0050] Under the protection of nitrogen atmosphere, dissolve 0.1 mol of imidazole in 100 mL of dichlorom...

Embodiment 3

[0058] 1. Synthesis of intermediate neopentyl glycol phosphorus oxychloride

[0059] Add 0.3mol of neopentyl glycol to a three-necked flask equipped with a spherical condenser, thermometer and magnetic stirring device, then add 150mL of dichloromethane as a solvent, stir to completely dissolve neopentyl glycol in the solvent, and keep the temperature at 3°C , then add 0.33mol phosphorus oxychloride dropwise, after the dropwise addition, the temperature is raised to 55°C, and the reaction is continued for 5h until no hydrogen chloride is released; after the reaction is completed, cool to room temperature, and distill off the solvent and unreacted trichloride under reduced pressure Oxyphosphorus, washed three times with n-hexane, and vacuum-dried to obtain the intermediate neopentyl glycol phosphorus oxychloride.

[0060] 2. Preparation of phosphorus nitrogen flame retardant

[0061] Under the protection of nitrogen atmosphere, dissolve 0.15 mol of imidazole in 150 mL of dichlo...

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Abstract

The invention discloses a novel phosphorus-nitrogen type flame retardant and a preparation method thereof, and relates to the technical field of flame retardants, and the structural formula of the phosphorus-nitrogen type flame retardant is as shown in the formula I. The preparation method of the phosphorus-nitrogen type flame retardant comprises the following steps: reacting an intermediate neopentyl glycol phosphoryl chloride with imidazole, cooling to room temperature after the reaction is completed, and carrying out suction filtration, water washing, reduced pressure rotary evaporation and drying to obtain the phosphorus-nitrogen type flame retardant; and blending the phosphorus-nitrogen flame retardant solution and the ripened viscose liquid to prepare a flame-retardant viscose spinning solution, forming in a coagulating bath, and drafting, washing and drying to obtain the phosphorus-nitrogen flame-retardant viscose fiber. The phosphorus-nitrogen type flame retardant prepared by the invention contains a nitrogen element, can play a flame retardant role when a condensed phase and a gas phase are used, and is simple in synthesis process, and is halogen-free, formaldehyde-free, environment-friendly and pollution-free; the prepared phosphorus-nitrogen type flame-retardant viscose fiber overcomes the defect that the existing viscose fiber is easy to burn, avoids the problems of poor durability, serious strength damage and the like, and improves the flame retardance of the viscose fiber.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a novel nitrogen-phosphorus flame retardant and its preparation method and application. Background technique [0002] At present, viscose fiber occupies an important position in regenerated cellulose fibers and is a major variety widely used in regenerated cellulose fibers. Its raw material sources are wide, the cost is low, and the processing technology is mature. In addition, viscose fiber has the moisture absorption and air permeability of cotton fiber, better spinnability than other regenerated cellulose fibers, and has excellent properties such as soft hand feeling and easy bleaching and dyeing. However, traditional viscose fiber does not have flame retardancy, and its limiting oxygen The index is only about 17%, which is extremely flammable. With the increasing application of viscose fibers in various industries, the fire hazards caused by viscose fibers are beco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574D01F2/08
CPCC07F9/65742D01F2/08
Inventor 朱平张晓云蒋之铭
Owner QINGDAO UNIV
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