Preparation method of triethyl phosphate

A technology of triethyl phosphate and absolute ethanol, which is applied in the chemical industry, can solve problems such as high production cost, high equipment requirements, and product damage, and achieve the effects of low production cost, reduced side reactions, and improved efficiency

Active Publication Date: 2012-09-19
雅克(上海)化工新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the production of triethyl phosphate mainly adopts the process of reacting phosphorus oxychloride and dehydrated alcohol under reduced pressure, such as Chinese patent 021524394 and Chinese patent application 2011100857020, but the following problems generally exist: one, phosphorus oxychloride and ethanol In the later stage of the reaction, the activity of phosphorus oxychloride decreases, and the method of raising the temperature is generally adopted to promote the complete reaction. However, raising the temperature will accelerate the acidolysis or hydrolysis of triethyl phosphate, which is not conducive to the improvement of the yield.
2. There is a small amount of water in the reaction system. Triethyl phosphate...

Method used

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  • Preparation method of triethyl phosphate
  • Preparation method of triethyl phosphate
  • Preparation method of triethyl phosphate

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Embodiment 1: 276g dehydrated alcohol, 4.2g anhydrous CuCl Join in the reactor that thermometer, constant pressure dropping funnel, mechanical stirring and decompression system are housed, start stirring and decompression device, make under ice bath condition When the temperature in the bottle drops below 5°C, start to add a mixture of 153g of phosphorus oxychloride and 1.5g of phosphorus pentachloride dropwise for 5 hours; after the addition, the temperature is raised to 30°C and kept for 3 hours. It is 2000Pa; continue to heat up to 70°C, and remove excess ethanol and part of hydrogen chloride at 500 Pa for 1 hour; then cool down to room temperature, normal pressure and under cooling conditions, feed ammonia gas while stirring until the pH value of the system 6-7, press filtration to remove the generated ammonium chloride to obtain crude triethyl phosphate. The crude product was rectified at 100 Pa to obtain triethyl phosphate product, 162 g of the product, with a pur...

Embodiment 2

[0019] Embodiment 2: 230g absolute ethanol, anhydrous MgCl22g are joined in the reaction kettle that thermometer, constant pressure dropping funnel, mechanical stirring and decompression system are housed, start stirring and decompression device, under ice bath condition make in bottle When the temperature drops below 5°C, start to drop a mixture of 153g of phosphorus oxychloride and 0.75g of phosphorus pentachloride for 4 hours; after the dropwise addition, raise the temperature to 25°C and keep it warm for 3 hours, and the system pressure during the whole process is 1000Pa Continue to heat up to 70°C, remove excess ethanol and part of hydrogen chloride at 100 Pa for 1.5 hours; then drop to room temperature, normal pressure and under cooling conditions, feed ammonia gas while stirring until the pH of the system is 6-7, press filter to remove the generated ammonium chloride to obtain crude triethyl phosphate. The crude product was rectified at 50 Pa to obtain triethyl phosphat...

Embodiment 3

[0020] Embodiment 3: 184g dehydrated alcohol, TiCl4 6.7g are joined in the reaction kettle that thermometer, constant pressure dropping funnel, mechanical stirring and decompression system are housed, start stirring and decompression device, under the condition of ice bath, make in the bottle When the temperature drops below 5°C, start to add a mixture of 153g of phosphorus oxychloride and 3g of phosphorus pentachloride dropwise, and the dropwise addition time is 4.5h; after the dropwise addition, the temperature is raised to 35°C and kept for 2h, and the system pressure is 1500Pa during the whole process ; continue to heat up to 70 ° C, remove excess ethanol and part of hydrogen chloride at 800 Pa for 1 h; then lower to room temperature, normal pressure and under cooling conditions, feed ammonia gas while stirring until the pH of the system is 6 -7, remove the generated ammonium chloride by pressure filtration to obtain the crude product of triethyl phosphate. The crude produ...

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Abstract

A preparation method of triethyl phosphate belongs to the field of chemical industry. After phosphorus oxychloride and absolute ethyl alcohol are subjected to low-pressure esterification reaction, excessive absolute ethyl alcohol and partial chlorine hydride are sequentially removed under reduced pressure, residual chlorine hydride is removed under normal pressure and rectification is carried out under reduced pressure to obtain the finished product of triethyl phosphate. With the addition of a catalyst, the temperature of esterification reaction is lowered and the reaction speed is increased, namely, the temperature is lowered to 25 to 35 DEG C from almost 50 DEG C before, and after excessive absolute ethyl alcohol is removed, ammonia is added for neutralization to remove chlorine hydride without water introduction, thus avoiding hydrolyzing triethyl phosphate; and the entire process is simple, high in yield and low in production cost.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for preparing triethyl phosphate. Background technique [0002] Triethyl phosphate (TEP for short) is a colorless and transparent liquid chemical product with a high boiling point and good solubility. It is widely used as a solvent, plasticizer and softener in the rubber and plastic industry; it is also prepared from pesticides. It can be used as a stabilizer for pesticides and as a plant growth regulator; in recent years, the country has become more and more strict with fire control requirements, chemical materials, building materials, interior decoration, electronic products, transportation, aerospace communications, etc. All walks of life have higher and higher requirements for flame retardancy. As an efficient flame retardant, triethyl phosphate occupies a place in the flame retardant market due to its good compatibility with substrates. [0003] At present, the pro...

Claims

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Application Information

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IPC IPC(8): C07F9/11
Inventor 沈琦褚昭宁瞿小新杨建军
Owner 雅克(上海)化工新材料有限公司
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