A kind of preparation method of highly hydrophilic flame-retardant polyester fiber

A flame retardant polyester, high hydrophilic technology, applied in the direction of one-component copolyester rayon, melt spinning, stretch spinning, etc., to achieve a small amount of addition, reduce the generation of diethylene glycol, and reduce the residence time Effect

Active Publication Date: 2015-10-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the use of sorbitol to prepare polyester for micro-modification.

Method used

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  • A kind of preparation method of highly hydrophilic flame-retardant polyester fiber
  • A kind of preparation method of highly hydrophilic flame-retardant polyester fiber
  • A kind of preparation method of highly hydrophilic flame-retardant polyester fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046]

[0047] The copolymerization flame retardant CEPPA is mixed with ethylene glycol in a molar ratio of 1:1.2, and the reaction is carried out at 100° C. for 1 hour to obtain the reaction product CEPPA-EG. Tetraethoxysilane (TEOS) was mixed with ethylene glycol in a molar ratio of 1:4 and reacted under the action of catalyst HCl to obtain a tetrakis (2-hydroxyethyl) orthosilicic acid solution. The terephthalic acid and the ethylene glycol slurry were mixed in a molar ratio of 1:1.05 to prepare a slurry. The prepared slurry was mixed with the catalyst tetrabutyl titanate and then added to the esterification reaction kettle to carry out the first esterification reaction. The first esterification reaction temperature was 225°C, the reaction time was 4h, and the relative pressure of the reaction was 0MPa. When the esterification reaction reached 82%, sorbitol and polyethylene glycol (PEG-200) were added to carry out the second esterification reaction. The second esterifica...

Embodiment 2

[0049]

[0050] The copolymerization flame retardant CEPPA was mixed with ethylene glycol in a molar ratio of 1:1.8, and reacted at 100° C. for 1 hour to obtain the reaction product CEPPA-EG. Mix the hydroxyl-terminated silicone oil with ethylene glycol in a molar ratio of 1:4.4, in the catalyst SiCl 4 Under the action of the reaction, a hydroxyl-terminated silicone oil-EG solution is obtained. The terephthalic acid and the ethylene glycol slurry are mixed in a molar ratio of 1:2.0 to prepare a slurry. The prepared slurry was mixed with ethylene glycol antimony, antioxidant 1010 and trimethyl phosphate, and then added to the esterification reactor to carry out the first esterification reaction. The temperature of the first esterification reaction was 250°C, and the reaction time was 0.5h. , the relative pressure of the reaction is 0.4MPa. When the esterification reaction reached 95%, 1,2-propanediol and polyethylene glycol (PEG-400) were added to carry out the second este...

Embodiment 3

[0052]

[0053] The copolymerization flame retardant CEPPA is mixed with 1,2 propylene glycol in a molar ratio of 1:2.0, and the reaction is carried out at 100° C. for 1 hour to obtain a reaction product CEPPA-1,2 propylene glycol. Tetraethoxysilane (TEOS) was mixed with ethylene glycol in a molar ratio of 1:4.6 in the catalyst Al(OC 2 H 5 ) 3 Under the action of the reaction, tetrakis (2-hydroxyethyl) orthosilicic acid solution is obtained. The terephthalic acid and the ethylene glycol slurry are mixed at a ratio of 1:1.6 to prepare a slurry. The prepared slurry is mixed with antimony trioxide and titanium dioxide mixture, antioxidant 168 and alkyl phosphoric acid diester, and then added to the esterification reactor to carry out the first esterification reaction. The first esterification reaction temperature is 240 ° C. The time was 3h, and the relative pressure of the reaction was 0.3MPa. When the esterification reaction reached 92%, 1,3-butanediol and polyethylene g...

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Abstract

The invention relates to a preparation method of high-hydrophilicity flame-retardant polyester fiber, which comprises the steps of (1) enabling a copolymer flame retardant to react with polyalcohol to obtain CEPPA (carboxethyl phenylphosphinic acid)-polyalcohol; (2) enabling hydroxyl-terminated siloxane to react with ethylene glycol in the presence of a catalyst to obtain a hydroxyl-terminated siloxane-ethylene glycol solution; (3) preparing slurry, and adding the prepared slurry into an esterification reaction kettle to perform a first esterification reaction; (4) when the quantity of the collected byproducts reaches 82-95% of the theoretical value, adding polyalcohol, sodium sulfo bis(hydroxyethyl) isophthalate (SIPE) and polyethylene glycol (PEG) to perform a second esterification reaction; (5) after the esterification reaction, adding the products obtained by the steps (1) and (2) into a reaction kettle, and after the condensation polymerization reaction, performing melt spinning to obtain the high-hydrophilicity flame-retardant polyester fiber. The limit oxygen index of the polyester fiber prepared by the method provided by the invention is over 30%, the moisture regain is 0.6-2.0%, and the fiber has relatively high moisture regain and is comfortable to wear.

Description

technical field [0001] The invention belongs to the field of preparation of flame-retardant fibers, in particular to a preparation method of highly hydrophilic flame-retardant polyester fibers. Background technique [0002] Since polyester and polyester fiber entered large-scale industrialization in the 1970s, the development speed is much faster than other synthetic materials and synthetic fibers. In 2011, the output of polyester fiber in my country was 27.95 million tons, accounting for about 83% of my country's chemical fiber output; It accounts for about 70% of the world's polyester fiber production. In the next 10 years, the world's polyester and polyester fiber will still maintain a growth rate of more than 3%, and polyester fiber will account for more than 60% of the world's total fiber products. The physical and mechanical properties of polyester fibers such as strength, wear resistance, resilience and dimensional stability are good, and can meet the needs of various...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/84C08G63/695C08G63/86C08G63/85D01D5/08D01D5/12D01D5/16D01D10/02
Inventor 王朝生方孝芬王华平李建武陈向玲
Owner DONGHUA UNIV
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