Method for preparing flame-resisting polyester in phosphorus series

A manufacturing method and technology of phosphorus-based flame retardants, which are applied in the field of manufacturing phosphorus-based flame-retardant copolyesters, can solve the problems of many reaction steps, long process routes, and many types of raw materials used, and achieve low cost and short process routes , the effect of fewer types of raw materials

Active Publication Date: 2005-01-12
SHAOXING SANLIDA TEXTILE FLAME RETARDANT NEW MATERIALS
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, these two methods all have the disadvantages of longer process routes, more reaction steps, too many types of raw materials, and the need for refining by-products.

Method used

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  • Method for preparing flame-resisting polyester in phosphorus series
  • Method for preparing flame-resisting polyester in phosphorus series

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1. The first step is to prepare a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant:

[0027] Take 45kg of commercially available 2-carboxyethylphenylphosphoric acid containing 14.5% of phosphorus and 2% of water, and 55kg of ethylene glycol, and add them to the esterification kettle, and gradually raise the temperature to 165°C under stirring, and carry out under normal pressure conditions. Esterification reaction, properly increase the reaction temperature to 170°C before the end of the esterification, collect the distilled water to reach 7.6kg, take the reaction product to measure the acid value to control and determine the desired reaction end point, the esterification rate is 90%, filter for later use . The product is a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant, which contains ethylene glycol p...

Embodiment 2

[0031] 1. The first step is to prepare a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol flame retardant: the method is the same as in Example 1.

[0032] 2. The second step, polymerization of flame retardant polyester:

[0033] Get 200kg of purified terephthalic acid (PTA) and 185kg of ethylene glycol (EG). The esterification process conditions and operation method are the same as in Example 1. After the esterification product is moved into the polycondensation tank, add the new flame retardant made in the first step 20kg of mixed solution (wherein containing EG6.9kg) is put in the polymerization kettle, and catalyst, auxiliary agent addition, polycondensation process condition and operating method are the same as embodiment one, obtain the required flame retardant polyester chip of the present invention. The phosphorus content in the flame-retardant polyester chip was 5560 ppm.

Embodiment 3

[0035] 1. The first step is to prepare the mixed solution of ethylene glycol propionate, ethylene glycol phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol:

[0036] Take 45kg of commercially available 2-carboxyethylphenylphosphoric acid containing 14.5% of phosphorus and 2% of water, and 55kg of ethylene glycol, and add them to the esterification kettle, and gradually raise the temperature to 165°C under stirring, and carry out under normal pressure conditions. Esterification reaction, properly increase the reaction temperature to 170°C before the end of the esterification, collect the distilled water to reach 6.1kg, take the reaction product to measure the acid value to control and determine the desired reaction end point, the esterification rate is 70%, filter for later use . The product is a mixture of ethylene glycol propionate-based phenylphosphate, 2-carboxyethylphenylphosphoric acid and ethylene glycol, which contains ethylene glycol propionate-ba...

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Abstract

In the prepairng method, fine p-phthalic acid, glycol, catalyst and assistant are used to carry out esterification; fire retardant mixed liquid containing glycol exter radical propionate-phenyl phosphorus acid glycol exter, 2-propyloic phenyl phosphorous acid and glycol is added before polymerization and after exterification; and conventional polycondensation process is applied to obtain fire resistant polyester chip.

Description

technical field [0001] The invention relates to the technical field of a new polymer synthesis halogen-free flame-retardant polymer material, in particular to a method for manufacturing a halogen-free phosphorus-based flame-retardant copolyester with good flame-retardant stability. Background technique [0002] With the enhancement of people's awareness of fire safety and the improvement of economic and technological level, in order to ensure the safety of people's lives and property, countries all over the world have imposed mandatory regulations on textiles and grade standards for flame-retardant textiles to varying degrees. The flame retardant performance of flame retardant textiles is mainly judged by checking the limiting oxygen index (LOI%) and damage degree of the product. 1 Grade" (LOI% ≥ 32%) and "flame retardant B 2 Grade" (32%>LOI%≥26%). [0003] There are two ways to obtain the flame retardant of textiles. One is post-treatment of textile flame retardant. T...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08K5/523
Inventor 李远明叶光斗
Owner SHAOXING SANLIDA TEXTILE FLAME RETARDANT NEW MATERIALS
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