Polyester industrial yarn solid-phase polymerization flame-retarding chain extender and preparing method thereof

A technology of polyester industrial yarn and solid-state polymerization, which is applied in the direction of chemical instruments and methods, single-component copolyester rayon, compounds of Group 5/15 elements of the periodic table, etc., can solve the difficulty of removing small molecules, Strict equipment requirements, high cost, etc., to achieve the effect of avoiding cumbersome process, mild reaction conditions, and improving intrinsic viscosity

Active Publication Date: 2012-08-01
JIANGSU HENGLI CHEM FIBER
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of polyester industrial yarn solid phase polymerization flame retardant chain extender and preparation method thereof, utilize PCl 3 in CHCl 3 / (CH 3 CH 2 O) 2 The solution is reacted with the phenolic hydroxyl group in 3-hydroxyphthalic anhydride to prepare a polyester industrial yarn chain extender containing acid anhydride groups and phosphorus elements in the molecular structure; the acid anhydride of the chain extender during solid-phase polymerization of polyester industrial yarn The polycondensation reaction between the group and the hydroxyl group in the PET molecule, and no small molecules are generated during the reaction process, which is beneficial to solve the problems of difficult removal of small molecules, high cost, and strict equipment requirements in the current solid-phase polymerization process of polyester industrial yarns; at the same time, in The phosphorus element introduced in the chain extender has a certain flame retardant function, so that the polyester industrial yarn obtained after chain extension has a certain flame retardant function

Method used

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  • Polyester industrial yarn solid-phase polymerization flame-retarding chain extender and preparing method thereof
  • Polyester industrial yarn solid-phase polymerization flame-retarding chain extender and preparing method thereof
  • Polyester industrial yarn solid-phase polymerization flame-retarding chain extender and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) CHCl 3 with (CH 3 CH 2 O) 2 The mixed solution is used as a solvent, and the solute is respectively prepared as PCl 3 The A solution and the B solution whose solute is 3-hydroxyphthalic anhydride; wherein, CHCl 3 with (CH 3 CH 2 O) 2 The volume ratio is 5:1, PCl in solution A 3 The molar volume concentration of is 0.3mol / L, and the molar volume concentration of 3-hydroxyphthalic anhydride in B solution is 0.05mol / L;

[0025] (2) Slowly add the B solution to the A solution system under the condition of 80°C and keep stirring. After the dropwise addition of the B solution, reflux at 80°C for 2 hours, and then evaporate at 60°C. is 30vol%, and then filtered to obtain the required flame retardant chain extender crude product; wherein, the volume ratio of A solution and B solution is 1: 3.5;

[0026] (3) The obtained flame retardant chain extender crude product is 5:1 CHCl with a volume ratio 3 with (CH 3 CH 2 O) 2 The mixed solution is used as a solvent, an...

Embodiment 2

[0028] (1) CHCl 3 with (CH 3 CH 2 O) 2 The mixed solution is used as a solvent, and the solute is respectively prepared as PCl 3 The A solution and the B solution whose solute is 3-hydroxyphthalic anhydride; wherein, CHCl 3 with (CH 3 CH 2 O) 2 The volume ratio is 8:1, PCl in solution A 3The molar volume concentration of is 0.2mol / L, and the molar volume concentration of 3-hydroxyphthalic anhydride in B solution is 0.05mol / L;

[0029] (2) Slowly add solution B to solution A at 60°C and stir continuously. After adding solution B dropwise, reflux at 60°C for 2 hours, and then evaporate at 60°C. is 30vol%, and then filtered to obtain the required flame retardant chain extender crude product; wherein, the volume ratio of A solution and B solution is 1: 3.5;

[0030] (3) The obtained flame retardant chain extender crude product is 5:1 CHCl with a volume ratio 3 with (CH 3 CH 2 O) 2 The mixed liquid is used as a solvent, and the desired flame-retardant chain extender cr...

Embodiment 3

[0032] (1) CHCl 3 with (CH 3 CH 2 O) 2 The mixed solution is used as a solvent, and the solute is respectively prepared as PCl 3 The A solution and the B solution whose solute is 3-hydroxyphthalic anhydride; wherein, CHCl 3 with (CH 3 CH 2 O) 2 The volume ratio is 8:1, PCl in solution A 3 The molar volume concentration of is 0.3mol / L, and the molar volume concentration of 3-hydroxyphthalic anhydride in B solution is 0.2mol / L;

[0033] (2) Slowly add solution B to solution A at 80°C and keep stirring. After adding solution B dropwise, reflux reaction at 80°C for 3 hours, and then evaporate at 60°C. 30vol%, and then filtered to obtain the required flame retardant chain extender crude product; wherein, the volume ratio of A solution and B solution is 1: 3.4;

[0034] (3) the obtained flame retardant type chain extender crude product is 8:1 CHCl with a volume ratio 3 with (CH 3 CH 2 O) 2 The mixed liquid is used as a solvent, and the required flame-retardant chain ext...

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Abstract

The invention provides a polyester industrial yarn solid-phase polymerization flame-retarding chain extender, which mainly comprises a double-end-group benzoic acid anhydride group serving as a chain extension group and a flame-retarding group containing phosphorus. Two acid anhydrides in a molecule can be used for reacting with hydroxyl in dacron molecules so that intrinsic viscosity of dacron is improved. Simultaneously, phosphorus is introduced into the molecule structure so that flame-retarding performance of dacron is improved. The invention further relates to a preparing method of the polyester industrial yarn solid-phase polymerization flame-retarding chain extender, which includes: (1) dissolving PCl3 into mixed solvent of CHCl3/(CH3CH2O)2, dropwise adding 3-hydroxy phthalic anhydride solution dissolved in the mixed solvent of CHCl3/(CH3CH2O)2, and performing heat preservation backflow reaction at certain temperature; and (2) evaporating a part of solvent at certain temperature after the reaction proceeds for a certain time, filtering the mixture which generates faint yellow sediments to obtain mixed solvent of CHCl3/(CH3CH2O)2 for solids, and recrystallizing to obtain required flame-retarding chain extension crystals.

Description

technical field [0001] The invention relates to a solid-phase polymerization flame-retardant chain extender for polyester industrial yarn and a preparation method thereof, in particular to a reactive double-terminal group, especially containing phthalic anhydride groups and phosphorus-containing groups , especially for improving the problem that the small molecules produced in the solid state polymerization process of polyester industrial yarns are difficult to remove, and conventional polyester industrial yarns do not have certain flame retardant properties. Mild reaction conditions are used to prepare flame retardant A solid phase polymerization chain extender for polyester industrial yarn. Background technique [0002] Polyester industrial yarn generally uses low-viscosity PET chips to make high-viscosity PET chips through solid-state polymerization, and then high-viscosity PET is a high-performance fiber produced at a spinning temperature above 300°C. It has excellent c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/80C07F9/655D01F6/84
Inventor 尹立新王朝生汤方明王华平王丽丽江振林杨大矛范晓兵
Owner JIANGSU HENGLI CHEM FIBER
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