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Method for removing Lewis acid ionic liquid catalyst in phosphate flame retardant product

A technology of liquid catalyst and phosphate ester, which is applied in chemical instruments and methods, phosphorus organic compounds, organic chemistry, etc. It can solve the problems of large acid value, cumbersome process, and unreported simplified methods, so as to ensure quality and solve acid reflux problem effect

Inactive Publication Date: 2020-02-21
南京师范大学镇江创新发展研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The post-processing of products has the problems of cumbersome process and high acid value.
[0005] According to the current published literature, the simplification of the post-treatment process for the synthesis of phosphate or phosphite flame retardant products has not been resolved, and the simplified method for the preparation of low-acid value and high-quality phosphate or phosphite flame retardants No report

Method used

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  • Method for removing Lewis acid ionic liquid catalyst in phosphate flame retardant product
  • Method for removing Lewis acid ionic liquid catalyst in phosphate flame retardant product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Phosphorus oxychloride and propylene oxide were used as raw materials, and tris(β-chloropropyl)phosphate (TCPP) was prepared by esterification reaction under the action of acidic ionic liquid catalyst. Add 15.4g of phosphorus oxychloride and 0.66g of aluminum trichloride into a four-necked flask equipped with a thermometer, reflux condenser, and electric stirrer, heat to 45-55°C, add 18.4g of propylene oxide dropwise, and keep the reaction temperature At 60-70°C. After the dropwise addition, continue the heat preservation reaction for 2 h, and distill off the unreacted substances under reduced pressure to obtain the crude product of TCPP.

[0028] Add dropwise 0.15g (equivalent to 0.45% of the total mass of TCPP product) water 60-70 in the reaction device o Stir at C for 0.5-1h, then add 0.068g Ca(OH) 2 (Equivalent to 0.2% of the total mass of TCPP products) Stir for 1-2 hours, blow nitrogen to remove water, and filter while hot to obtain low-acid value and low-moistu...

Embodiment 2

[0032] Phosphorus oxychloride and ethylene oxide are used as raw materials, and tris(β-chloroethyl)phosphate (TCEP) is prepared by esterification under the action of an acidic ionic liquid catalyst. Add 15.4g of phosphorus oxychloride and 0.57g of titanium tetrachloride into a four-necked flask equipped with a thermometer, reflux condenser, and electric stirrer, heat to 40-50°C, add 14.2g of ethylene oxide dropwise, and keep the reaction The temperature is 55-65°C. After the dropwise addition, the reaction was continued for 3 h, and the unreacted substances were removed by distillation under reduced pressure to obtain the crude product of TCEP.

[0033] Add 0.133g (equivalent to 0.45% of the total mass of TCEP product) water 55-65 in the reaction device o Stir at C for 0.5-1h, then add 0.0592g Ca(OH) 2 (Equivalent to 0.2% of the total mass of TCEP products) Stir for 1-2 hours, blow nitrogen to remove water, and filter while hot to obtain TCEP products with low acid value and...

Embodiment 3

[0037] Phosphorus oxychloride and epichlorohydrin are used as raw materials to obtain tris(2,3-dichloropropyl)phosphate (TDCPP) through esterification under the action of acidic ionic liquid catalyst. Add 15.4g of phosphorus oxychloride and 0.86g of aluminum trichloride into a four-necked flask equipped with a thermometer, reflux condenser, and electric stirrer, heat to 50-60°C, add 29.8g of epichlorohydrin dropwise, and keep the reaction The temperature was 70-80°C. After the dropwise addition, the reaction was continued for 3.5 hours, and the unreacted substances were distilled off under reduced pressure to obtain the crude product of TDCPP.

[0038] Add 0.120g (equivalent to 0.45% of the total mass of TDCPP product) water 70-80% in the reaction device o Stir at C for 0.5-1h, then add 0.0888g Ca(OH) 2 (Equivalent to 0.2% of the total mass of the TDCPP product) Stir for 1-2 hours, blow nitrogen to remove water, and filter while hot to obtain a low-acid value and low-moisture...

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Abstract

The invention relates to a method for removing a Lewis acid ionic liquid catalyst in a phosphate flame retardant product, wherein the method can remove a small amount of a Lewis acid ionic liquid catalyst in a phosphate product. The method comprises: carrying out an organic reaction under the action of a Lewis acid ionic liquid ([A]-x[Lewis acid]) (wherein A represents amine and a derivative thereof, imidazole and a derivative thereof or pyridine and a derivative thereof) catalyst to obtain a crude product, adding a certain amount of water into the reaction device, stirring for 0.5-1 h at thereaction temperature, adding a certain amount of a post-treatment agent, stirring for 1-2 h, blowing nitrogen to remove water, and filtering while hot to obtain a low-acid-value product (less than orequal to 0.05 mg KOH<-1>). According to the invention, the method effectively reduces the acid value of the product, and solves the problem of serious acid return after long-term placement of the product.

Description

technical field [0001] The invention relates to a treatment method for removing a small amount of Lewis ionic liquid catalyst in liquid flame retardant products to reduce the acid value of the product, in particular to a treatment method for reducing the acid value of phosphoric acid ester or phosphite flame retardants, avoiding a large amount of A green method that produces a large amount of industrial waste water by washing with water or alkali, so as to effectively simplify the post-treatment process of liquid flame retardant products and meet environmental protection requirements. Background technique [0002] Among liquid flame retardant products, phosphate ester or phosphite ester is widely used in polyurethane foam, epoxy resin, rubber, coating, polystyrene, cellulose resin, artificial leather, phenolic resin, soft PVC and other materials. For example, tris(β-chloropropyl) phosphate (TCPP) has excellent flame retardancy, plasticizing, moisture-proof, anti-static, anti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F9/141C07F9/142C07F9/145
CPCC07F9/091C07F9/1411C07F9/142C07F9/145
Inventor 职慧珍张继杨锦飞黄小冬
Owner 南京师范大学镇江创新发展研究院
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