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

A technology of copolyester and phosphorus-silicon, which is applied in the field of preparation of organic polymer compounds, can solve the problems of no phosphorus-silicon-fluorine flame-retardant copolyester resin, affecting the inherent properties of polyester materials, and poor flame-retardant effect. Achieve the effects of shortening production time and cycle, easy control of process conditions, and increasing char formation rate

Active Publication Date: 2014-01-08
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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  • Preparation method of flame-retardant copolyester film of phosphorus, silicon and fluorine
  • Preparation method of flame-retardant copolyester film of phosphorus, silicon and fluorine
  • Preparation method of flame-retardant copolyester film of phosphorus, silicon and fluorine

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The first step: under stirring at a speed of 60-120 rpm, 2000mol maleic anhydride, 3200mol of dihydroxy fluorosiloxane containing 3200mol of hydroxyl (hydroxyl mass content of 5%), 2020mol of DOPO, 10000mol of 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) One-time addition to the reactor with fractional distillation condenser, beating and mixing for 10-20 minutes, heating to 105±5℃ for simultaneous addition and esterification for 0.5-1 hour, The temperature is increased to 250±5°C to accelerate the completion of the esterification reaction, and the reaction is terminated when the effluent volume reaches more than 96% of the theoretical effluent volume.

[0036] The second step: Put the reaction material of the first step into the polycondensation reactor, stir at a speed of 1...

Embodiment 2

[0038] The first step: under stirring at a speed of 60-120 rpm, 2000mol of maleic anhydride, 3600mol of dihydroxy fluorosiloxane (hydroxyl mass content of 7%), 2020mol of DOPO, 10500mol of 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) One-time addition to the reactor with fractionating condenser, beating and mixing for 10-20 minutes, heating to 125 ± 5 ℃ for simultaneous addition The reaction between the formation and the esterification is 0.5 to 1 hour, and then the temperature is increased to 255±5°C to accelerate the completion of the esterification reaction. The reaction is terminated when the effluent volume reaches more than 96% of the theoretical effluent volume.

[0039] The second step: Put the reaction materials of the first step into th...

Embodiment 3

[0041] Step 1: Mix 2000mol of maleic anhydride, 4000mol of dihydroxy fluorosiloxane (hydroxyl mass content 8%), 2020mol of DOPO, and 11000mol of A mixture of phthalic acid and 2,6-naphthalenedicarboxylic acid (terephthalic acid: 2,6-naphthalenedicarboxylic acid = 6:1 molar ratio), 25000mol ethylene glycol, 1.0kg esterification catalyst (cobalt acetate: acetic acid Sodium: manganese acetate = 1:1:1 mass ratio), 0.9kg polycondensation catalyst antimony trioxide and 0.1kg stabilizer trimethyl phosphate, triphenyl phosphate = 1:1 mass ratio) one-time addition with fractionation In the reactor of the condenser, beating and mixing for 10-20 minutes, heating to 145±5℃ for simultaneous addition and esterification for 0.5-1 hour, and then heating to 250±5℃ to accelerate the completion of the esterification reaction. The reaction ends when the effluent volume reaches more than 96% of the theoretical effluent volume.

[0042] The second step: Put the reaction materials of the first step in...

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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 polymer 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 adopting the invention is suitable for the fields of electrical insulation, decorative inkjet advertising, various IC cards and magnetic cards. Background technique [0002] In the prior art, the flame retardant of polyester usually adopts two methods: physical addition of flame retardant or reactive flame retardant. Chinese patent ZL200910058655.3 discloses phosphorus-containing flame-retardant polyethylene terephthalate. The Chinese patent application 200610041495.8 discloses "Polyester with excellent flame-retardant properties and its preparation method", which adopts the copolymerization of silicon-containing monomer and polyethylene terephthalate to obtain a non-drip flame-retardant polyester. Because a ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/695B29C48/92
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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