Method for synthesizing phosphorus-containing polyester for fire retardant electronic packaging material

A technology of electronic packaging materials and synthesis methods, which is applied in the field of electronic packaging materials, can solve problems such as inability to realize continuous production, and achieve the effects of stable production, simple synthesis process, and easy control of conditions

Active Publication Date: 2008-11-19
天津凯华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

[0005] About the synthetic method of phosphorus-containing polyester, CN101065417A discloses a kind of method that the pre-esterification liquid of phosphorus-containing compound and ethylene glycol is added in polyhydric alcohol and polycarboxylic acid and carries out copolymerization, and this method must prepare phosphorylation liquid in advance , cannot achieve continuous production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Add 12.07g of ethylene glycol, 8.76g of 2-methyl 1,3 propanediol, and 233.26g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column, and condenser tube, heat and stir to melt Finally, add 5.69g of adipic acid, 110g of terephthalic acid, 6.47g of isophthalic acid, 133.45g of CEPPA, 202.28g of DDP and 0.6g of tetrabutyl titanate. Esterified water is distilled out. During the reaction process, the temperature of the distillation column is controlled not to be higher than 100°C, and then a segmented esterification reaction is carried out, heating at 180-220°C for 5 hours, heating at 220-240°C for 4 hours, and heating at 240-270°C React for 3-5 hours, when the acid value of the reaction system is less than 18mgKOH / g, carry out vacuum polycondensation, the vacuum degree is -0.05MPa, and the vacuuming time is 30min; when the acid value is between 2-5mgKOH / g, lower the temperature To 200°C, add 224.47g of trimellit...

Embodiment 2

[0038]Add 10.54g of ethylene glycol, 9.56g of 2-methyl 1,3 propanediol, and 254.46g of neopentyl glycol to a 1L four-neck flask equipped with a heating mantle, stirrer, thermometer, distillation column, and condenser tube, heat and stir to melt Finally, add 6.21g of adipic acid, 120g of terephthalic acid, 7.06g of isophthalic acid, 236.58g of CEPPA, 73.56g of DDP and 0.6g of tetrabutyl titanate. Esterified water is distilled out. During the reaction, the temperature of the distillation column is controlled not to be higher than 100°C, and then a segmented esterification reaction is carried out, heating at 180-220°C for 5 hours, heating at 220-240°C for 4 hours, and heating at 240-270°C React for 3 to 5 hours. When the acid value of the reaction system is less than 18mgKOH / g, vacuum polycondensation is carried out. The vacuum degree is -0.05MPa, and the vacuuming time is 30 minutes; 200°C, add 228.56g of trimellitic anhydride to block, react at 170-190°C for 1.5h, then vacuumiz...

Embodiment 3

[0041] Add 8.23g of ethylene glycol, 9.96g of 2-methyl 1,3 propanediol, and 265.07g of neopentyl glycol into a 1L four-neck flask equipped with a heating mantle, agitator, thermometer, distillation column and condenser, heat and stir to melt Finally, add 6.47g of adipic acid, 125g of terephthalic acid, 7.35g of isophthalic acid, 293.82g of CEPPA and 0.6g of tetrabutyl titanate. The water is distilled out, and the temperature of the distillation column is controlled not to be higher than 100°C during the reaction, and then a segmented esterification reaction is carried out, and the reaction is heated at 180-220°C for 5 hours, 220-240°C for 4 hours, and 240-270°C for 3-3 hours. 5h, when the acid value of the reaction system is less than 18mgKOH / g, conduct vacuum polycondensation, the vacuum degree is -0.05MPa, and the vacuuming time is 30min; when the acid value is between 2 and 5mgKOH / g, cool down to 200°C , adding 221.07g of trimellitic anhydride to end capping, reacting at 17...

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Abstract

The invention relates to a method for synthesizing phosphorous polyester used for fire-retardant electronic packaging materials, aiming to obtain the polyester with high fire resistance to solve the fire-retardant problem of the electronic packaging materials. The method for synthesizing the phosphorous polyester comprises the following steps that: firstly, polylol is added into a four-mouth flask, and the temperature is increased to over 100 DEG C so that the polylol is stirred to be melt; secondly, polyatomic acid / estolide, reactive phosphorous compound and catalyst are respectively added into the molten polylol; the esterification reaction begins and esterifying water is generated and distilled off; thirdly, vacuum-pumping is performed for polycondensation when the esterification rate reaches over 95 percent; fourthly, end capping reagent is added and then the finished phosphorous polyester can be prepared, wherein, the acid value range is between 50 and 250 KOH / g, and the fusing temperature range is between 60 and 130 DEG C. The phosphorous polyester prepared by the method is used for the fire-retardant electronic packaging materials and can realize non-halogenation of the electronic packaging materials.

Description

technical field [0001] The invention belongs to the field of electronic packaging materials, in particular to a method for synthesizing phosphorus-containing polyester used for flame-retardant electronic packaging materials. Background technique [0002] Epoxy resin is one of the most widely used matrix resins in polymer-based composite materials. It has excellent adhesion, chemical corrosion resistance, electrical insulation properties, mechanical properties, and easy processing, low shrinkage, and small linear expansion coefficient. And low cost and other advantages, widely used in the packaging of electronic components such as varistors, ceramic capacitors, diodes, and triodes. Since the limiting oxygen index (LOI) of epoxy resin is low, only 19.5, it is a flammable substance, so it needs to be treated with flame retardancy. Usually, the way to improve the flame retardancy of epoxy resin is to introduce a halogen-containing flame retardant into the epoxy resin, and coope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/78C08G63/692
Inventor 沈纪洋席小悦
Owner 天津凯华绝缘材料股份有限公司
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