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Continuous preparation method of substituted diaryl phosphate compound

A technology of diarylphosphoric acid and compound, which is applied in the field of continuous preparation of substituted diarylphosphoric acid compounds, can solve the problems of low production efficiency, long reaction time, low safety and the like, and achieves high production efficiency and short reaction time. , the effect of high safety

Pending Publication Date: 2022-01-07
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide a continuous preparation method of substituted diaryl phosphoric acid compounds, which solves the problems of long reaction time, low production efficiency, complicated operation and low safety in the prior art

Method used

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  • Continuous preparation method of substituted diaryl phosphate compound
  • Continuous preparation method of substituted diaryl phosphate compound
  • Continuous preparation method of substituted diaryl phosphate compound

Examples

Experimental program
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Effect test

Embodiment 1

[0039]

[0040] Weigh 2,2'-methylene-bis(4,6-di-tert-butyl)phenol (0.025mol, 10.63g) and triethylamine (0.15mol, 20.85mL), dissolve with 80mL toluene and load in a raw material tank. Phosphorus oxychloride (0.0275 mol, 2.56 mL) was dissolved with 40 mL of toluene and charged in another raw material tank. The reaction solution in the two raw material tanks, under the action of the feed pump, continuously enters the vibrating reactor filled with spherical stainless steel internals with an inner diameter of 5mm and a length of 8m through the Y-shaped mixer. The vibration mode is pneumatic and the frequency is 10Hz. The temperature is controlled at 10°C, normal pressure, the residence time is 180s, and the material is discharged into the Y-type mixer; 30mL of water and triethylamine (0.075mol, 10.42mL) are placed in a raw material tank, under the action of the feed pump Enter the Y-type mixer, mix with the discharge material and continuously enter the vibrating reactor filled ...

Embodiment 2

[0042] Weigh 2,2'-methylene-bis(4,6-di-tert-butyl)phenol (0.025mol, 10.63g) and triethylamine (0.15mol, 20.85mL), dissolve with 80mL toluene and load in a raw material tank. Phosphorus oxychloride (0.0275 mol, 2.56 mL) was dissolved with 40 mL of toluene and charged in another raw material tank. The reaction liquid in the two raw material tanks, under the action of the feed pump, continuously enters the vibrating reactor filled with cylindrical stainless steel internals with an inner diameter of 5 mm and a length of 8 m through a Y-shaped mixer. The vibration mode is electromagnetic vibration and the frequency is 10 Hz. , the reaction temperature is controlled at 10°C, normal pressure, the residence time is 180s, and the discharge enters the Y-shaped mixer; 30mL of water and triethylamine (0.075mol, 10.42mL) are placed in a raw material tank, and the feed pump Under the action, it enters the Y-type mixer, mixes with the discharge material and continuously enters the vibrating...

Embodiment 3

[0044] Weigh 2,2'-methylene-bis(4,6-di-tert-butyl)phenol (0.025mol, 10.63g) and triethylamine (0.15mol, 20.85mL), dissolve in 100mL of toluene and load in a raw material tank. Phosphorus oxychloride (0.0275 mol, 2.56 mL) was dissolved with 50 mL of toluene and charged in another raw material tank. The reaction solution in the two raw material tanks, under the action of the feed pump, continuously enters the vibrating reactor with an inner diameter of 8 mm and a length of 10 m filled with vertical spiral stainless steel internals through a Y-shaped mixer. The reactor remains static and the reaction temperature Controlled at 10°C, normal pressure, residence time of 180s, the discharge enters the Y-shaped mixer; 30mL of water and triethylamine (0.075mol, 10.42mL) are placed in a raw material tank, and enter under the action of the feed pump Y-shaped mixer, mixed with the output material and continuously enters the vibrating reactor with an inner diameter of 8mm and a length of 2...

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Abstract

The invention discloses a continuous preparation method of a substituted diaryl phosphate compound, which comprises the steps disclosed in the invention; the preparation method of the substituted diaryl phosphate compound in a continuous reactor provided by the invention has the characteristics of short reaction time, mild reaction conditions, high purity, few byproducts, high yield, large output and the like, the utilization rate of raw materials is very high, the technical process is more green, environment-friendly, economical and efficient, the product yield is up to 99% or above, and the product purity is up to 99.9% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a continuous preparation method of substituted diaryl phosphoric acid compounds. Background technique [0002] Substituted diaryl phosphate nucleating agent is a widely used polymer material modification additive, which can change the crystallinity of crystalline polymer and accelerate its crystallization by providing crystal nuclei to promote crystallization and refine the grain size Speed, thereby improving the rigidity, heat distortion temperature, dimensional stability, transparency and surface gloss of the product. Substituted diaryl phosphate nucleating agents have been one of the most active product categories in the development of polymer modification additives since the 1990s. In the past 30 years, new structures have emerged one after another, but by analyzing their chemical structures, it can be found that these new structures of organophosphate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/527
CPCC07F9/65744C08K5/527
Inventor 辛忠万力姚翰林辛玉成
Owner EAST CHINA UNIV OF SCI & TECH
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