Preparation method of cationic dyeable flame-retardant polyester resin

A technology of cationic dyes and flame-retardant polyesters, which is applied in the field of preparation of organic polymer compounds, and can solve problems such as high addition of flame retardants, increased dyeing capacity, poor flame retardancy, etc.

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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention provides a flame-retardant copolyester resin dyeable by normal pressure cationic dyes and a manufacturing method thereof, which not only solves the problems of high flame retardant addition, low melting point and poor flame retardancy of the copolyester resin, Sulfonate-based isophthalic acid (or its derivatives) can effectively reduce the regularity of the molecular structure of copolyester, increase the dyeing capacity, and realize the normal pressure dyeing of cationic dyes for flame-retardant polyester fibers

Method used

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  • Preparation method of cationic dyeable flame-retardant polyester resin
  • Preparation method of cationic dyeable flame-retardant polyester resin
  • Preparation method of cationic dyeable flame-retardant polyester resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Take 1.91kg of hydroxyethylphenyl hypophosphorous acid, 10kg of ethylene glycol and 0.2g of composite catalyst (antimony acetate: zinc acetate = 3:1) and place them in reactor A, stir evenly and heat up to 175°C, under the condition of pressure 60kPa , and discharged after 4 hours of esterification to obtain a flame retardant esterification liquid.

[0073] Take 1.2kg of dimethyl isophthalate-5-sodium sulfonate, 4.8kg of ethylene glycol and 0.06g of composite catalyst (antimony acetate:magnesium acetate=2:1), put them in reaction kettle B, stir evenly and heat up to At 165°C, under the condition of a pressure of 55kPa, the material was discharged after the transesterification reaction for 4 hours to obtain a bishydroxyethyl isophthalate-5-sodium sulfonate solution.

[0074] Take 40kg of terephthalic acid and 20.9kg of ethylene glycol and place them in reactor C, stir evenly, raise the temperature to 248°C, and carry out the esterification reaction for 3 hours. After the...

Embodiment 2

[0076] Take 2.34kg of hydroxyethylphenyl hypophosphorous acid, 10kg of ethylene glycol and 0.23g of composite catalyst (calcium acetate: manganese acetate = 2:1) and place them in reactor A, stir evenly and heat up to 155°C, under the condition of pressure 65kPa , and discharged after 4.5 hours of esterification to obtain a flame retardant esterification solution.

[0077] Take 0.4kg of dimethyl isophthalate-5-sodium sulfonate, 1.2kg of ethylene glycol and 0.08g of composite catalyst (calcium acetate: antimony acetate = 1:1), put them in reaction kettle B, stir evenly and heat up to Under the condition of 175°C and a pressure of 50kPa, the material was discharged after the transesterification reaction for 3 hours to obtain a bishydroxyethyl isophthalate-5-sodium sulfonate solution.

[0078] Take 40kg of terephthalic acid and 19.0kg of ethylene glycol and place them in reactor C, stir, raise the temperature to 255°C, and carry out esterification reaction for 3 hours. After the ...

Embodiment 3

[0080] Take 2.94kg of hydroxyethylphenyl hypophosphorous acid, 10kg of ethylene glycol and 0.25g of composite catalyst (manganese acetate: cobalt acetate = 3:1) in reactor A, stir evenly and heat up to 160°C, under the condition of pressure 45kPa , and discharged after 3 hours of esterification to obtain a flame retardant esterification liquid.

[0081] Take 0.20kg of isophthalic acid-5-sodium sulfonate, 3.6kg of ethylene glycol and 0.07g of composite catalyst (zinc acetate: cobalt acetate = 1:1), put them in reaction kettle B, stir evenly and heat up to 160°C, Under the condition of a pressure of 40kPa, after 3.5 hours of the transesterification reaction, the material was discharged to obtain a bishydroxyethyl isophthalate-5-sodium sulfonate solution.

[0082] Take 40kg of terephthalic acid and 18.5kg of ethylene glycol and place them in reactor C, stir, raise the temperature to 250°C, and carry out the esterification reaction for 2.5 hours. After the esterification reaction ...

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Abstract

The invention discloses a preparation method of cationic dyeable flame-retardant polyester resin. The manufacturing method is characterized by comprising the following steps: performing an esterification reaction on a halogen-free copolymerized phosphorus-based flame retardant, ethylene glycol and a composite catalyst to prepare an esterification solution of the halogen-free copolymerized flame retardant; performing ester exchange reaction on sulfoisophthalic acid dimethyl ester and the ethylene glycol to prepare a sulfonate-based bis(hydroxyethyl) isophthalate solution; performing an esterification reaction on terephthalic acid (or dimethyl terephthalate), the ethylene glycol and auxiliaries, then adding a catalyst, a stabilizer, the auxiliaries, the esterification solution of the phosphorus-based flame retardant (or a prepolymer solution of the phosphorus-based flame retardant) and the sulfonate-based bis(hydroxyethyl) isophthalate solution, performing condensation polymerization reaction, and cooling and dicing after the end of reaction to prepare the cationic dyeable flame-retardant polyester resin. The cationic dyeable flame-retardant polyester resin prepared by the method disclosed by the invention has the characteristics of good spinnability, polyester fiber cationic dye boiling dyeing under normal pressure conditions, complete chromatogram and strong dye adhesion.

Description

technical field [0001] The invention belongs to the preparation of organic macromolecular compounds, and relates to a method for manufacturing a cationic dye-dyeable flame-retardant polyester resin. The cationic dye-dyeable flame-retardant polyester resin prepared by the invention is mainly used in the manufacture of cationic dye-dyeable flame-retardant polyester fibers under normal pressure. Background technique [0002] With the development of high-rise buildings, aviation and shipping, and the improvement of people's awareness of fire protection, the market demand for flame-retardant polyester is increasing. At the same time, the requirements for color and color fastness of flame-retardant polyester fibers are gradually increasing. There are three methods of flame retardant modification of polyester materials: blending, copolymerization and finishing. The material is flame retardant treated by blending. The amount of flame retardant added is large, which has a great impac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/685C08G63/82
Inventor 梁倩倩江涌刘健飞除维敏
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