Method for preparing modified cellulose fire-retardant fiber through reaction extrusion

A technology of reactive extrusion and flame-retardant fibers, which is applied to the manufacture of artificial filaments in cellulose solution, fire-resistant and flame-retardant filaments, stretch spinning, etc., and can solve the problems of shortening the service life of flame-retardant fibers and flame-retardant spinning Long liquid time, low spinning process efficiency and other problems, to achieve the effect of prolonging the service life, stable and reliable product quality, and high production efficiency

Inactive Publication Date: 2013-06-12
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two preparation methods of flame retardant cellulose fibers also adopt the blending method. Although the spinning process used can make the flame retardant evenly dispersed without adding other additives, the flame retardant and cellulose molecules are physically separated. Effects (such as van der Waals force, intermolecular force) are combined, so that with the increase of fiber use time and washing times, the loss of flame retardant is serious, and its content in the fiber decreases; the flame retardant effect of the fiber also decreases, and the flame retardant The burning time is shortened, resulting in a shortened service life of flame-retardant fibers
Moreover, in the patent CN101608348, the wet or dry-wet spinning process is adopted, and the time for mixing and dissolving to prepare the flame-retardant spinning solution is too long, so that the efficiency of the entire spinning process is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Stir the pulverized cotton pulp with a degree of polymerization of 1000, O, O-diethylphosphoryl thiochloride, acid-binding agent and [BMIM]Cl ionic liquid in a high-speed mixer at a ratio of 10:10:5:90 , and then fed into a twin-screw extruder with an aspect ratio of 40, through the reaction extrusion method, the dissolution, reaction and extrusion of cellulose are carried out simultaneously, that is, the as-spun filaments of modified fibers are obtained. The temperature of the feeding section, the melting section, the metering section and the spinning die of the extruder were 60°C, 80°C, 100°C and 120°C respectively, and the screw speed was 20 rpm. Stretch the above-mentioned as-spun silk, wherein the stretching temperature is 100°C, and the stretching ratio is 0.5 times. After stretching, the fiber obtained by washing, heat setting and crimping is a modified cellulose flame-retardant fiber, specifically cellulose O, O-Diethylphosphorothioate.

[0036] The obtained ce...

Embodiment 2

[0038] Stir the pulverized wood pulp with a degree of polymerization of 600, O, O-dibutyl thiophosphoryl chloride, acid-binding agent and [AMIM]Cl ionic liquid in a high-speed mixer according to the ratio of 15:12:6:85 , and then fed into a twin-screw extruder with an aspect ratio of 60, through the reaction extrusion method, the dissolution, reaction and extrusion of cellulose are carried out simultaneously, that is, the as-spun silk of the modified fiber is obtained. The temperature of the feeding section, the melting section, the metering section and the spinning die of the extruder were respectively 100°C, 110°C, 120°C and 130°C, and the screw speed was 30 rpm. Stretch the above as-spun silk, wherein the stretching temperature is 140°C, and the stretching ratio is 1.5 times. After stretching, the fiber obtained by washing, heat setting and crimping is a modified cellulose flame-retardant fiber, specifically cellulose O, O-Diethylphosphorothioate.

[0039] The obtained cel...

Embodiment 3

[0041] Bamboo pulp with a degree of polymerization of 400, O, O-diisopropylphosphoryl thiochloride, acid-binding agent and [EMIM]Ac ionic liquid were stirred evenly in a high-speed mixer according to the ratio of 25:20:8:75, Then it is fed into a twin-screw extruder with an aspect ratio of 80, and the cellulose is dissolved, reacted and extruded simultaneously through the reaction extrusion method, that is, the as-spun silk of the modified fiber is obtained. The temperatures of the feeding section, the melting section, the metering section and the spinning die of the extruder were respectively 100°C, 120°C, 140°C and 160°C, and the screw speed was 10 rpm. Stretch the above-mentioned as-spun silk, wherein the stretching temperature is 120°C, and the stretching ratio is 3 times. After stretching, the fiber obtained by washing, heat setting and crimping is a modified cellulose flame-retardant fiber, specifically cellulose O, O-Diethylphosphorothioate.

[0042] The obtained cellu...

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Abstract

The invention discloses a method for preparing a modified cellulose fire-retardant fiber through reaction extrusion, and the method comprises the following steps of: 1. preparing a fire retardant, cellulose, a solvent and an acid-binding agent into a mixture according to a certain mass ratio, wherein the fire retardant is a novel phosphorus-based fire retardant, the cellulose is one of wood pulp, cotton pulp or bamboo pulp, the solvent is ion liquid, the acid-binding agent is potassium carbonate, the proportion is as follows: the mass ratio of the acid-binding agent to the fire retardant is 0.1-0.5:1, the mass ratio of the fire retardant to the cellulose is 0.5-2:1, and the mass ratio of the cellulose to the solvent is 10-25:90-75; 2. feeding the mixture into a double-screw extruder, and synchronously carrying out dissolution, reaction and extrusion of the cellulose through a reaction extrusion method to obtain the freshly formed filament of modified cellulose; and 3. stretching, washing, thermoforming and curling the freshly formed filament to prepare the modified cellulose fire-retardant fiber. The modified cellulose fire-retardant fiber obtained through the method disclosed by the invention has the advantages of no halogen, environmental friendliness without pollution and outstanding flame-retardant effect.

Description

technical field [0001] The invention relates to a preparation technology of modified cellulose flame retardant fiber, in particular to a method for preparing modified cellulose flame retardant fiber by reactive extrusion. Background technique [0002] Cellulose is the most abundant natural polymer material bestowed by nature to human beings. It is not only rich in sources, but also a renewable resource. Processing and utilization of cellulosic materials is of positive significance to the world's circular economy and sustainable development. However, because cellulose materials are highly flammable in case of fire, the limiting oxygen index is only about 17, which limits its use in the fields of life and industry. Therefore, the production of flame-retardant cellulose materials to prevent fires has become a social problem that cannot be ignored, and has attracted more and more attention. [0003] At present, many countries in the world have put forward specific requirements...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F2/02D01F1/07D01D1/04D01D5/14
Inventor 程博闻陆飞宋俊纪秀杰王乐军高磊
Owner TIANJIN POLYTECHNIC UNIV
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