Cardanol-based phosphatefire-retardant plasticizer and preparation method thereof

A technology of cardanol-based phosphate and cardanol-based diethyl phosphate, applied in the field of preparation of environmentally friendly bio-based flame-retardant plasticizers, to achieve the effects of reducing production costs, shortening reaction time, and reducing production energy consumption

Inactive Publication Date: 2015-05-13
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Studies have shown that cardanol and its derivatives can be used as plasticizers for rubber or PVC, and have achieved good plasticizing effects; however, the method of preparing flame-retardant plasticizers from cardanol has not been reported at home and abroad.

Method used

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  • Cardanol-based phosphatefire-retardant plasticizer and preparation method thereof
  • Cardanol-based phosphatefire-retardant plasticizer and preparation method thereof
  • Cardanol-based phosphatefire-retardant plasticizer and preparation method thereof

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Effect test

preparation example Construction

[0026] A preparation method of cardanol-based phosphate flame-retardant plasticizer, the steps are:

[0027] Step 1: Take 10-20g of cardanol, 6-8g of diethyl chlorophosphate, and 1.2-2.5g of acid-binding agent, add them to 20-40mL of solvent, mix and stir to heat up to 60-80°C, and react for 2-4 hours; Filtration and vacuum distillation treatment to obtain cardanyl phenolic diethyl phosphate; Step 2: Weigh 5 to 10 g cardanyl phenolic diethyl phosphate, peroxyphosphotungstate phase transfer catalyst (accounting for cardanyl phenolic diethyl phosphate 2% to 5% of the mass), stir evenly with 10 to 30mL solvent, heat the reaction system to 40 to 50°C, add a peroxygen source dropwise, and react at 55 to 70°C for 0.5 to 3 hours to obtain epoxy cardanyl diethyl phosphate The crude ester is filtered, washed and dehydrated to obtain the finished epoxy cardanol-based diethyl phosphate plasticizer.

[0028] The acid-binding agent is one or two or more of sodium hydroxide, potassium carb...

Embodiment 1

[0036] Put 2.5mmol tungstic acid in a 50mL beaker, add 20mmol H 2 o 2, stirred vigorously until the pale yellow precipitate disappeared, added 1.5mmol phosphoric acid (89% concentration) dropwise, and 5mL distilled water, raised the temperature to 60°C, and stirred for 30min to obtain a colorless and transparent solution; Dissolve methyl ammonium chloride in 20mL ethyl acetate, mix and add dropwise to the above solution, drop it within 5min, a small amount of light yellow precipitate appears, continue stirring for about 30min, until the phase of docosyl peroxyphosphotungstate The transfer catalyst polymerized and precipitated at the oil-water two-phase interface; the catalyst was taken out by filtration, rinsed with deionized water until the washing liquid was neutral, placed in a vacuum drying oven, fully dried and ground at room temperature.

Embodiment 2

[0038] Put 2mmol tungstic acid in a 50mL beaker, add 15mmol H 2 o 2 , stirred vigorously until the light yellow precipitate disappeared, then added dropwise 0.5mmol phosphoric acid (89% concentration) and 2mL distilled water, raised the temperature to 60°C, and stirred for 30min to obtain a colorless and transparent solution; take 1mmol octadecyldimethyl Dissolve ammonium chloride in 15mL of dichloromethane, mix and add dropwise to the above solution, within 5 minutes, a small amount of light yellow precipitate appears, continue to stir for about 30 minutes, until the octadecyl peroxyphosphotungstate phase transfer catalyst is in the Polymerization and precipitation occurred at the oil-water two-phase interface; the catalyst was taken out by filtration, washed with deionized water until the washing liquid was neutral, the catalyst was placed in a vacuum drying oven, fully dried and ground at room temperature.

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Abstract

The invention discloses a cardanol-based phosphatefire-retardant plasticizer and a preparation method thereof. The preparation method comprises the following steps: with cardanol and diethyl chlorophosphate as main raw materials, carrying out substitution reaction in the presence of an acid binding agent to synthesize cardanol-based diethyl phosphate; further with cardanol-based phosphoric acid as a raw material, in the presence of a peracetic phosphotungstate phase transfer catalyst, adding a peracetic source dropwise for epoxidation to prepare crude epoxy cardanol-based diethyl phosphate, and filtering, washing and dehydration to obtain a finished epoxy cardanol-based glycidyl ether plasticizer. According to the cardanol-based phosphatefire-retardant plasticizer and the preparation method disclosed by the invention, as the cardanol is taken as the raw material, the cost is low, and the source is wide; the preparation process is simple, the energy consumption is low; the product is low in toxicity, is environmentally friendly, is capable of endowing a polymer substrate with excellent flame retardancy and flexibility and has good application prospect.

Description

technical field [0001] The invention belongs to the technical field of preparation of environment-friendly bio-based flame-retardant plasticizers, and in particular relates to a method for preparing epoxy cardanol-based diethyl phosphate plasticizers using cardanol as a raw material. Background technique [0002] Phosphate esters are a class of widely used flame retardant plasticizers, the most commonly used ones include trioctyl phosphate (TOP), triphenyl phosphate (TPP) and tributyl phosphate (TBP). However, these products generally have shortcomings such as high toxicity, low plasticizing efficiency, general plasticizing performance, and poor low-temperature performance, which greatly limit their application fields. In response to this problem, a series of low-toxic phosphate plasticizers have been developed at home and abroad in recent years, such as cumyl phosphate (IPP), which is colorless, odorless, low-toxic and efficient, and vinyl chloride nitrocellulose Synthetic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/521C07F9/655C08L27/06
Inventor 陈洁蒋剑春聂小安黄金瑞李科王义刚
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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