Method for synthesizing reactive halogen-free flame-retardant unsaturated polyester resin

The technology of a polyester resin and a synthesis method, which is applied in the field of preparation of polymer compounds, can solve the problems of increased flexibility of products, sticky surface of resin castings, large amount of escape, etc., and achieves improved mechanical properties, good product quality, and improved preparation. simple craftsmanship

Active Publication Date: 2011-09-14
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If this kind of reactive flame retardant is not pre-treated with diols and is added to the reactor with diols, dibasic acids and other substances for direct reaction, it is difficult for the phosphoric acid groups on CEPPA or HMPPA to participate in the reaction, resulting in the acid value of the system It is difficult to descend, and the surface of the resin casting body will have serious stickiness
The addition of additive-type flame retardants has a great impact on the mechanical properties of unsaturated polyesters. Additive-type organic flame retardants also have a problem of dissipation, which will increase with the increase of ambient temperature and affect the resistance of unsaturated polyester. flame retardant effect; adding styrene crosslinking agent, styrene has a wick effect, which makes the flame retardant effect of unsaturated polyester resin unsatisfactory
To sum up, the existing reaction and addition of mixed phosphorus-containing flame-retardant unsaturated polyester resins have toughening properties due to most additive-type organic flame retardants, which will increase the flexibility of the product and decrease the rigidity, while the organic flame retardants will also increase the toughness. There is a problem of dissipation. The ambient temperature has a great influence on dissipation. The higher the temperature, the greater the dissipation, which affects the flame retardant effect.

Method used

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  • Method for synthesizing reactive halogen-free flame-retardant unsaturated polyester resin
  • Method for synthesizing reactive halogen-free flame-retardant unsaturated polyester resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Add 100 grams of ethylene glycol and 80 grams of CEPPA into a 1000ml three-neck flask equipped with a stirrer, thermocouple and rectification tower, and react at 140°C to 160°C for 3 to 5 hours. The prepolymer 1 was obtained after reacting at ℃ for 2-4 hours, and cooled down to room temperature for use.

[0031] (2) Add 80 grams of 1,2-propanediol, 20 grams of diethylene glycol, 210 grams of maleic anhydride, and 40 grams of phthalate in another 1000ml three-necked flask with a stirrer, a thermocouple and a rectifying tower Acid anhydride, 0.2 g of dibutyltin oxide, 20 g of diphenyl dihydroxysilane, 0.07 g of hydroquinone, heat up to 140°C, keep warm for 1 hour, gradually heat up to 200°C in 6-8 hours, keep warm for 2-4 Add all the prepolymer 1 obtained in (1), gradually heat up to 200°C, react for 1 hour and then vacuumize under reduced pressure, the vacuum degree is -0.093MPa, until the acid value of the resin drops to 30-40mgKOH / g for the reaction At the end poi...

Embodiment 2

[0033] (1) Add 140 grams of ethylene glycol, 10 grams of neopentyl glycol, and 200 grams of CEPPA in a 1000ml three-necked flask equipped with a stirrer, a thermocouple and a rectification tower, and react at 140°C to 160°C for 3 to 5 hours. - 0.093MPa vacuum degree, react at 160°C for 2 to 4 hours to obtain prepolymer 1, cool down to room temperature for use.

[0034] (2) Add 150 grams of 1,2-propanediol, 300 grams of maleic anhydride, 20 grams of isophthalic acid, and 10 grams of phthalic acid in another 1000ml three-necked flask with a stirrer, thermocouple and rectification tower Acid anhydride, 20 grams of adipic acid, 0.3 grams of dibutyltin oxide, 0.2 grams of butyltin dilaurate, 70 grams of diphenyl dihydroxysilane, 0.2 grams of hydroquinone, heat up to 140 ° C, keep warm for 1 hour, use 6 ~ Gradually raise the temperature to 200°C for 8 hours, keep it warm for 2 to 4 hours, add all the prepolymer 1 obtained in (1), gradually heat up to 200°C, react for 1 hour and then...

Embodiment 3

[0036](1) Add 130 grams of ethylene glycol, 10 grams of diethylene glycol, and 150 grams of CEPPA into a 1000ml three-neck flask equipped with a stirrer, a thermocouple and a rectification tower, and react at 140°C to 160°C for 3 to 5 hours. - 0.093MPa vacuum degree, react at 160°C for 2 to 4 hours to obtain prepolymer 1, cool down to room temperature for use.

[0037] (2) Add 140 grams of 1,2-propanediol, 10 grams of neopentyl glycol, 320 grams of maleic anhydride, 0.4 grams of dibutyl oxide in another 1000ml three-necked flask with a stirrer, thermocouple and rectification tower Tin, 23 grams of diphenyldihydroxysilane, 0.1 gram of hydroquinone, heating up to 140 ° C, heat preservation for 1 hour, gradually warming up to 200 ° C in 6 to 8 hours, heat preservation for 2 to 4 hours, adding (1) obtained All prepolymers 1, gradually heated up to 200°C, and after 1 hour of reaction, depressurized and vacuumed, with a vacuum degree of -0.093MPa, until the acid value of the resin d...

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Abstract

The invention discloses a method for synthesizing reactive halogen-free flame-retardant unsaturated polyester resin. The method is characterized by taking dihydric alcohol, dibasic acid or dibasic acid anhydride, reactive phosphorus flame retardants such as 2- carboxyethyl (phenyl) phosphinic acid and phenyl hydroxymethyl phosphinic acid, and reactive silicon flame retardants such as dihydroxy diphenyl silane and dihydroxy dimethyl silane as basic materials, conducting esterification and polycondensation under the conditions of catalysts such as dibutyltin oxide and sodium acetate, and then adding diluent, thus preparing the halogen-free flame-retardant unsaturated polyester resin. The resin prepared by the method is especially applicable to the production of unsaturated polyester resin moulding compounds, glass fiber reinforced plastics and electrical plastic products, can meet the requirements of products on flame retarding and lightweight and has good properties.

Description

technical field [0001] The invention belongs to a preparation method of a polymer compound, and relates to a synthesis method of a reactive halogen-free flame-retardant unsaturated polyester resin. The reactive halogen-free flame retardant unsaturated polyester resin prepared by the method is especially suitable for the manufacture of flame retardant light unsaturated polyester molding compound or composite materials such as glass fiber reinforced plastics and electrical plastic products. Background technique [0002] The rapid development of the world economy and the great progress of society are all faced with the strategic problem of how to balance the exhaustion of resources, environmental protection and sustainable development, and the technology related to the molding compound and glass fiber reinforced plastic products with a large market volume related to the present invention The development trend of the market is environmentally friendly, halogen-free, flame-retard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/01C08G63/695C08G63/78
Inventor 李先德曾彬夏平原
Owner SICHUAN DONGFANG INSULATING MATERIAL
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