Method for preparing phosphor system halogen-free flame-proof copolymerization polyester

A copolyester and phosphorus-based technology, which is applied in the field of polymer compound preparation, can solve the problem of difficulty in obtaining high flame-retardant grade co-polymerized flame-retardant polyester, limiting the increase of the real content of flame retardants, and failing to achieve halogen-free flame retardants. Combustible products and other issues, to achieve the effect of increasing the effective addition amount, improving the reaction performance, and increasing the flame retardant effect

Active Publication Date: 2009-08-19
四川东方绝缘材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods all use organophosphorus flame retardants for pretreatment in different ways and then add the polyester reaction system in the esterification or polycondensation stage to obtain a copolymerized flame retardant polyester; although the above methods better improve the flame retardant chip However, due to the influence of polymerization conditions and the activity of various reactants, this type of polyester limits the increase of the real content of flame retardants, and it is difficult to obtain high flame-retardant grade co

Method used

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  • Method for preparing phosphor system halogen-free flame-proof copolymerization polyester
  • Method for preparing phosphor system halogen-free flame-proof copolymerization polyester
  • Method for preparing phosphor system halogen-free flame-proof copolymerization polyester

Examples

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Effect test

Embodiment 1

[0029] A preparation method of phosphorus-based halogen-free flame-retardant copolyester, comprising the following steps:

[0030] Take 2.1kg of hydroxymethylphenyl hypophosphorous acid and 3.2kg of ethylene glycol, put them into the esterification kettle, raise the temperature to 155°C and fully stir, carry out the esterification reaction under 60kpa pressure for 5 hours, and the esterification reaction reaches more than 95%. The material is filtered, and the filtrate is the esterification liquid for subsequent use;

[0031] Take 25kg of terephthalic acid (PTA), 13kg of ethylene glycol (EG), and 29g of pentaerythritol, stir and mix well, heat to 250°C to 255°C for esterification for 3 hours, and when the esterification reaches 90% or more, Add the aforementioned standby hydroxymethylphenylphosphinic acid pre-esterification solution, then add 20g of catalyst antimony acetate and 20g of stabilizer phosphoric acid and stir evenly, gradually depressurize to below 100pa and carry ...

Embodiment 2

[0033] A preparation method of phosphorus-based halogen-free flame-retardant copolyester, comprising the following steps:

[0034] The preparation method of this embodiment is different from Example 1 in that: when preparing the flame retardant pre-esterification liquid, the addition amount of hydroxymethylphenyl hypophosphorous acid is 1.8kg, and the addition amount of ethylene glycol is 2.75kg. The amount of phosphorus (P) added to the flame-retardant polyester chips was 11220ppm. Others are identical with embodiment 1, omitted.

Embodiment 3

[0036] A preparation method of phosphorus-based halogen-free flame-retardant copolyester, comprising the following steps:

[0037] Take 2.1kg of hydroxymethylphenyl hypophosphorous acid and 3.5kg of ethylene glycol into the esterification kettle, polycondense at 155°C and pressure below 1000Pa for 3 to 4 hours, discharge and filter for later use.

[0038] Take 25kg of terephthalic acid (PTA), 13kg of ethylene glycol (EG), and 29g of pentaerythritol, stir and mix well, heat to 250°C-255°C for esterification reaction for 2-4 hours, and the esterification reaction is over 90%. , add the aforementioned standby hydroxymethylphenylphosphinate prepolymer, add 16g of catalyst antimony trioxide and 25g of stabilizer trimethyl phosphate, stir evenly, gradually reduce the pressure to below 100pa, and carry out polycondensation at a temperature of 285°C Reaction, polymerization reaction for 2.5 to 3 hours, and the phosphorus-based halogen-free flame-retardant copolyester is obtained after d...

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PUM

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Abstract

The invention relates to a method for preparing phosphorus halogen-free flame retardant copolyester. The method is characterized in that halogen-free phosphoric copolymerized flame retardant and glycol are mixed to carry out esterification reaction for 4 to 6 hours under the temperature of 140-210 DEG C and the pressure of 40-70Kpa and then are filtered; flame-retardant esterified product solution is prepared from the filtrate; dimethyl terephthalate, the glycol and promoter are mixed to carry out ester exchange reaction for 2 to 4 hours under the temperature of 160-240 DEG C; after the reaction, the flame-retardant esterified product solution is added, and catalyst and stabilizing agent are added to carry out polyreaction for 2.5 to 4 hours under the temperature of 240-290 DEG C and the pressure of 100Pa; and the phosphorus halogen-free flame retardant copolyester is prepared after discharging the material. Polyester slice can be used as raw material for producing film with flame retardance of grade 94UL V-O or grade VTM-O (collectively called grade VO), flame retardant fibre with flame retardance of grade I or above and grade VO flame retardant plastic product, and the polyester slice has excellent flame retardance.

Description

technical field [0001] The invention belongs to a preparation method of a polymer compound obtained by forming a carboxylate bond on a polymer main chain, and relates to a preparation method of a phosphorus-based halogen-free flame-retardant copolyester. The polyester chips prepared by this method can be used as raw materials for the production of films with a flame-retardant performance of 94UL V-0 level or VTM-O level (collectively referred to as V0 level), flame-retardant fibers of level I and above, and V0-level flame-retardant plastic products. . Background technique [0002] Since the 1970s, the research and application development of flame-retardant polyester has become increasingly active all over the world, and various flame-retardant polyester technologies have come out continuously. After decades of development, flame retardant technology is mainly divided into blending, copolymerization, and post-treatment technology on the one hand, and can be divided into halo...

Claims

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Application Information

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IPC IPC(8): C08G63/78C08G63/692C08G63/183
Inventor 梁倩倩胡俊祥
Owner 四川东方绝缘材料股份有限公司
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