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Vinyl phosphate flame retardant and preparation method thereof

A technology of vinyl phosphate and flame retardant, which is applied in the field of flame retardants, can solve problems such as not being disclosed, and achieve the effects of easy operation, environmental protection, and good application prospects

Inactive Publication Date: 2020-07-03
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But do not disclose above-mentioned problem solving technical scheme temporarily in existing document

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of vinyl phosphate flame retardant, which includes the following steps: In a 500ml four-necked flask equipped with nitrogen inlet and outlet and stirring rotor, 9.82g phenylphosphoryl dichloride and 0.105mol pyridine are added as catalysts In 80ml of dichloromethane, add 13.66g of hydroxyethyl methacrylate dissolved in 80ml of dichloromethane dropwise within 1 hour under slow stirring at 0°C. After the addition is complete, raise the temperature to 30°C, and then react for 8h , That is, until there is no HCl released, the reaction is over; stand still, the product is rotary evaporated in a rotary evaporator for 25 minutes to remove the solvent, the distilled product is washed three times with saturated brine, and then dried with anhydrous magnesium sulfate for 12 hours, and finally The colorless liquid obtained by suction filtration is the target product vinyl phosphate, and the measured yield is 91%.

Embodiment 2

[0026] A preparation method of vinyl phosphate flame retardant, which includes the following steps: In a 500ml four-necked flask equipped with nitrogen inlet and outlet and stirring rotor, 9.82g phenylphosphoryl dichloride and 0.105mol pyridine are added as catalysts In 80ml of ether, 12.19g of 2-hydroxyethyl acrylate dissolved in 80ml of ether was added dropwise within 1 hour at 10°C under slow stirring. After the addition was completed, the temperature was raised to 35°C. After reacting for 10 hours, wait until no HCl is released, the reaction is over; let stand, the product is rotary evaporated in a rotary evaporator for 30 minutes to remove the solvent, the remaining product of distillation is washed with saturated brine three times, and then dried with anhydrous magnesium sulfate for 10 hours Finally, the colorless liquid obtained by suction filtration is the target product vinyl phosphate, and the measured yield is 87%.

Embodiment 3

[0028] A preparation method of vinyl phosphate flame retardant, which includes the following steps: In a 500ml four-necked flask equipped with nitrogen inlet and outlet and stirring rotor, 11.20g phenylphosphoryl dichloride and 0.21mol triethylamine are used as catalysts Add to 80ml of tetrahydrofuran, add 30.28g of 2-hydroxypropyl methacrylate dissolved in 100ml of tetrahydrofuran dropwise within 1 hour at 15°C under slow stirring. After the addition is complete, raise the temperature to 50°C, then React for 8h, wait until no HCl is released, the reaction is over; let stand, the product is rotatory-evaporated in a rotary evaporator for 39 minutes to remove the solvent, the remaining product of the distillation is washed three times with saturated brine, and then dried with anhydrous calcium chloride for 13 hours Finally, the colorless liquid obtained by suction filtration is the target product vinyl phosphate, and the measured yield is 85%.

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Abstract

The invention discloses a vinyl phosphate flame retardant, wherein phenylphosphonic dichloride and alkyl acrylate are subjected to a reaction in one of dichloromethane, diethyl ether or tetrahydrofuran serving as a solvent under the action of a catalyst triethylamine or pyridine to generate a final target product, wherein the two chlorides of phenylphosphonic dichloride are disubstituted by alkylacrylate to obtain the product phenylphosphane alkene ester. According to the invention, the vinyl phosphate flame retardant does not contain halogen, is non-toxic, is beneficial to environmental protection, has high thermal stability and high charring property, is a reactive organophosphorus flame retardant, can be widely applied to preparation of various acrylic acid and acrylate flame-retardantcoating material emulsions, does not affect the adhesion, weather resistance and other properties of coating materials after being added into the coating materials, and can achieve high flame-retardant effect under the condition that the addition amount of the flame-retardant agent in the coating material is small.

Description

Technical field [0001] The invention relates to the field of flame retardants, in particular to a vinyl phosphate flame retardant containing phosphorous vinyl monomers and a preparation method thereof. Background technique [0002] Acrylic emulsion has been widely used as a film-forming base material for water-based coating materials due to its excellent film-forming properties, flexibility and environmental protection, and is used in technical fields such as coatings, adhesives, textile printing and dyeing, and daily chemical industries. However, acrylate polymers are extremely flammable, which severely limits their application in fields with higher flame retardancy requirements. Additive flame retardants are generally added in a relatively large amount, and the compatibility of the external flame retardant with the emulsion is not good, which has a greater impact on the performance of the emulsion itself and the mechanical properties and appearance of the prepared coating. The...

Claims

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Application Information

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IPC IPC(8): C09D5/18C09D133/04C07F9/40
CPCC09D5/18C09D133/04C07F9/4075
Inventor 谢德龙朱苗苗郑睿智陈人杰梅毅
Owner KUNMING UNIV OF SCI & TECH
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