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Preparation method of flame-retardant copolyester film of phosphorus, silicon and fluorine

A technology of copolyester and phosphosilicon, which is applied in the field of preparation of organic polymer compounds, can solve the problems of not finding phosphosilicon fluorine flame retardant copolyester resin, affecting the inherent properties of polyester materials, and having poor flame retardant effect, etc. Achieve the effect of shortening production time and cycle, easy control of process conditions, and improving carbon formation rate

Active Publication Date: 2012-08-15
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

In the prior art, DOPO is applied in polyester materials by means of physical addition. Since there is no cross-linking, it is easy to migrate, the flame retardant effect is not good, and the dosage is large, which affects the inherent properties of polyester materials.
Phosphorus silicon fluorine flame retardant copolyester resin and its film products with DOPO structure have not been found

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The first step: under stirring at a speed of 60-120 rpm, mix 2000mol of maleic anhydride, dihydroxyfluorosiloxane containing 3200mol of hydroxyl groups (the content of hydroxyl mass is 5%), 2020mol of DOPO, 10000mol of para Phthalic acid, 18000mol ethylene glycol, 0.3kg esterification catalyst antimony acetate, 1.6kg polycondensation catalyst tetrabutyl titanate and 0.6kg stabilizer (bisphenol A phosphite: triphenyl phosphite: triethyl phosphate =1:2:1 mass ratio) into the reactor with fractionation condenser at one time, beating and mixing for 10-20 minutes, heating to 105±5°C for simultaneous addition and esterification for 0.5-1 hour, Then raise the temperature to 250±5°C to accelerate the completion of the esterification reaction, and end the reaction when the water output reaches more than 96% of the theoretical water output.

[0036] The second step: Put the reaction material of the first step into the polycondensation reactor, stir at a speed of 15-60 rpm, raise ...

Embodiment 2

[0038]The first step: Stirring at a speed of 60-120 rpm, mix 2000mol maleic anhydride, dihydroxyfluorosiloxane containing 3600mol hydroxyl (hydroxyl mass content 7%), 2020mol DOPO, 10500mol para Phthalic acid, 22000mol ethylene glycol, 0.8kg esterification catalyst (cobalt acetate: sodium acetate = 2:1 mass ratio), 0.6kg polycondensation catalyst ethylene glycol antimony and 0.9kg stabilizer (bisphenol A phosphite: Catechol phosphate: triethyl phosphate = 2:1:4 (mass ratio) into the reactor with fractionation condenser at one time, beating and stirring for 10 to 20 minutes, heating to 125±5°C for simultaneous addition Formation and esterification reaction for 0.5 to 1 hour, then raise the temperature to 255±5°C to accelerate the completion of the esterification reaction, and end the reaction when the water output reaches more than 96% of the theoretical water output.

[0039] The second step: Put the reaction materials of the first step into the polycondensation reactor, stir ...

Embodiment 3

[0041] The first step: under stirring at a speed of 60-120 rpm, mix 2000mol of maleic anhydride, dihydroxyfluorosiloxane containing 4000mol of hydroxyl groups (the content of hydroxyl mass is 8%), 2020mol of DOPO, 11000mol of para A mixture of phthalic acid and 2,6-naphthalene dicarboxylic acid (terephthalic acid: 2,6-naphthalene dicarboxylic acid = 6:1 molar ratio), 25000mol ethylene glycol, 1.0kg esterification catalyst (cobalt acetate: acetic acid Sodium: manganese acetate = 1:1:1 mass ratio), 0.9 kg polycondensation catalyst antimony trioxide and 0.1 kg stabilizer trimethyl phosphate, triphenyl phosphate = 1:1 mass ratio) one-time addition with fractionation In the reactor of the condenser, beating and stirring for 10 to 20 minutes, heating to 145±5°C for simultaneous addition and esterification for 0.5 to 1 hour, and then heating to 250±5°C to accelerate the completion of the esterification reaction. The reaction ends when the water output reaches more than 96% of the the...

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Abstract

The invention discloses a preparation method of a flame-retardant copolyester film of phosphorus, silicon and fluorine. The preparation method is characterized by comprising the steps of: preparing flame-retardant copolyester sections of phosphorus, silicon and fluorine from maleic anhydride, dihydroxy fluorine silicone, DOPO (9-10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), terephthalic acid and ethylene glycol by addition, esterification and polycondensation reaction in the presence of an esterification catalyst, a polycondensation catalyst and a stabilizing agent; and mixing the prepared flame-retardant copolyester sections of phosphorus, silicon and fluorine with a polyester section, carrying out melt extrusion by an extruder and preparing the flame-retardant copolyester film product of phosphorus, silicon and fluorine by longitudinally drawing, laterally drawing and hot setting treatment. The preparation method disclosed by the invention is simple in reaction process, strong in operability, easy in technological condition control and low in production cost, and shortens the production time and cycle of multivariate copolymerization synthesis; and the flame-retardant property of the product can be up to VTM-0 level.

Description

technical field [0001] The invention belongs to the preparation of organic macromolecular compounds, and relates to a preparation method of a phosphorus-silicon-fluorine flame-retardant copolyester film. The phosphorus-silicon-fluorine flame-retardant copolyester film prepared by the invention is suitable for the fields of electrical insulation, decorative inkjet advertisements, various IC cards and magnetic cards. Background technique [0002] In the prior art, the flame retardancy of polyester usually adopts two ways of physically adding flame retardants or reactive flame retardants. Chinese patent ZL200910058655.3 discloses phosphorus-containing flame-retardant polyethylene terephthalate. However, Chinese patent application 200610041495.8 discloses "Polyester with Excellent Flame Retardant Performance and Preparation Method thereof", which adopts silicon-containing monomers to copolymerize with polyethylene terephthalate to obtain a non-dripping flame retardant polyester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/02C08G63/695C08G63/78B29C47/92B29C55/14B29C48/92
CPCB29C48/0022B29C48/04B29C48/92B29C2948/92704B29C2948/92923
Inventor 李建学胡俊祥梁倩倩唐安斌
Owner 四川东方绝缘材料股份有限公司
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