A kind of phosphorus nitrogen flame retardant and its preparation method and application

A technology of flame retardant and phosphorus nitrogen, which is applied in the field of flame retardants, can solve the problems of poor hand feeling and resistance to washing, and achieve the effects of small loss of strength, easy operation, environmental protection and pollution-free application

Active Publication Date: 2022-06-21
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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  • A kind of phosphorus nitrogen flame retardant and its preparation method and application
  • A kind of phosphorus nitrogen flame retardant and its preparation method and application
  • A kind of phosphorus nitrogen flame retardant and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Synthetic intermediate neopentyl glycol phosphorus oxychloride

[0036] In a three-necked flask equipped with a spherical condenser, a thermometer and a magnetic stirring device, first add 0.1 mol of neopentyl glycol, then add 50 mL of dichloromethane as a solvent, and stir to completely dissolve the neopentyl glycol in the solvent, keeping the temperature at 3 °C , and then dropwise added 0.11mol phosphorus oxychloride, after the dropwise addition, the temperature was raised to 55 ° C, and the reaction was continued for 5 h until no hydrogen chloride was released; after the reaction was completed, it was cooled to room temperature, and the solvent and unreacted trichloride were removed by distillation under reduced pressure. Phosphorus oxide, washed three times with n-hexane, and dried in vacuum, which is the intermediate neopentyl glycol phosphorus oxychloride.

[0037] 2. Preparation of phosphorus nitrogen flame retardant

[0038] Under the protection of nitrogen...

Embodiment 2

[0047] 1. Synthetic intermediate neopentyl glycol phosphorus oxychloride

[0048] In a three-necked flask equipped with a spherical condenser, a thermometer and a magnetic stirring device, first add 0.2 mol of neopentyl glycol, then add 100 mL of dichloromethane as a solvent, stir to make the neopentyl glycol completely dissolve in the solvent, and keep the temperature at 3 °C , and then dropwise added 0.22mol phosphorus oxychloride, after the dropwise addition, the temperature was raised to 55 ° C, and the reaction was continued for 5 h until no hydrogen chloride was released; after the reaction was completed, it was cooled to room temperature, and the solvent and unreacted trichloride were removed by distillation under reduced pressure. Phosphorus oxide, washed three times with n-hexane, and dried in vacuum, which is the intermediate neopentyl glycol phosphorus oxychloride.

[0049] 2. Preparation of phosphorus nitrogen flame retardant

[0050] Under the protection of nitro...

Embodiment 3

[0058] 1. Synthetic intermediate neopentyl glycol phosphorus oxychloride

[0059] In a three-necked flask equipped with a spherical condenser, a thermometer and a magnetic stirring device, first add 0.3 mol of neopentyl glycol, then add 150 mL of dichloromethane as a solvent, stir to make the neopentyl glycol completely dissolve in the solvent, and keep the temperature at 3 °C , and then dropwise added 0.33mol phosphorus oxychloride, after the dropwise addition, the temperature was raised to 55 ° C, and the reaction was continued for 5 h until no hydrogen chloride was released; after the reaction was completed, it was cooled to room temperature, and the solvent and unreacted trichloride were removed by distillation under reduced pressure. Phosphorus oxide, washed three times with n-hexane, and dried in vacuum, which is the intermediate neopentyl glycol phosphorus oxychloride.

[0060] 2. Preparation of phosphorus nitrogen flame retardant

[0061] Under the protection of nitro...

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PUM

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Abstract

The invention discloses a novel phosphorus-nitrogen flame retardant and a preparation method thereof, and relates to the technical field of flame retardant technology. The structural formula of the phosphorus-nitrogen flame retardant of the invention is shown in Formula I. The preparation method of the phosphorus-nitrogen type flame retardant is to react the intermediate neopentyl glycol phosphorus oxychloride with imidazole, cool to room temperature after the reaction is completed, filter with suction, wash with water, rotary evaporate under reduced pressure, and dry to obtain the phosphorus-nitrogen type flame retardant . Phosphorus-nitrogen flame retardant solution is blended with mature viscose solution to make flame-retardant viscose spinning solution, which is put into coagulation bath for forming, and then drawn, washed, and dried to obtain phosphorus-nitrogen flame-retardant viscose fiber. The phosphorus-nitrogen type flame retardant prepared by the present invention contains nitrogen elements, can play a flame-retardant effect in the condensed phase and gas phase, has a simple synthesis process, has no halogen and formaldehyde in the structure, and is environmentally friendly and pollution-free; the prepared phosphorus-nitrogen type flame retardant The viscose fiber eliminates the shortcomings of the existing viscose fiber that are extremely flammable, avoids problems such as poor durability and serious damage to strength, and improves the flame retardancy 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 a preparation method and application thereof. Background technique [0002] At present, viscose fiber occupies an important position in regenerated cellulose fiber, and is a major variety widely used in regenerated cellulose fiber. Its raw material source is 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 feel and easy bleaching and dyeing. However, traditional viscose fiber does not have flame retardancy, and its limited oxygen The index is only about 17%, and it is extremely flammable. With the increasing application of viscose fiber in various industries, the fire hazard caused by viscose fiber is becoming...

Claims

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Application Information

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Patent Type & Authority Patents(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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