Process for preparing trioctyl phosphate by sodium alkoxide method

A technology for the preparation of trioctyl phosphate, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of increased separation difficulty, environmental pollution, and high production costs. Achieve the effect of improving the utilization rate of raw materials, reducing production costs, and reducing the difficulty of processing

Inactive Publication Date: 2010-11-17
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the decompression method mainly has the following defects: a large amount of HCl gas is produced during the reaction process, causing non-negligible environmental pollution; HCl is very soluble in water, forming hydrochloric acid, which corrodes equipment and pipelines; dioctyl phosphate reacts to generate phosphoric acid The reaction of trioctyl ester is a control step, the reaction speed is slow, and a large number of side reactions will occur. Under the condition that there are by-products, an emulsified layer will be formed on the interface when separating TOP, which will increase the difficulty of separation; the reaction will be slow under the condition of no catalyst , is difficult to apply to industrial production; adding catalyst can speed up the reaction, but the introduction of catalyst makes it difficult to recycle unreacted octanol, and the production cost is high

Method used

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  • Process for preparing trioctyl phosphate by sodium alkoxide method
  • Process for preparing trioctyl phosphate by sodium alkoxide method
  • Process for preparing trioctyl phosphate by sodium alkoxide method

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Weigh 250g of octanol and pour it into a four-necked reaction flask (500ml), weigh 11.06g of sodium metal, the molar fraction of sodium alkoxide is 25%, cut the sodium into pieces and put it into the reaction flask. Start the electric stirrer, heat with an electric heating mantle, and control the temperature to about 90°C. Weigh the corresponding stoichiometric amount of phosphorus oxychloride and place it in a constant pressure dropping funnel, and insert the funnel into a four-necked bottle. When the temperature of the reaction solution in the four-necked bottle is lower than 40°C, start to add phosphorus oxychloride dropwise, and control the dropping rate of phosphorus oxychloride (40-50 drops / min). Do not exceed 90°C. After the dropwise addition, the electric heating mantle was turned on to heat the reaction solution. The temperature was raised to 130°C over a period of 40 minutes, and the reaction was carried out at this temperature for 3 hours. Slowly lower the...

Embodiment 2

[0019] Weigh 250g of octanol and pour it into a four-necked reaction flask (500ml), weigh 6.64g of sodium metal, the molar fraction of sodium alkoxide is 15%, cut the sodium into pieces and put it into the reaction flask. Start the electric stirrer, heat with an electric heating mantle, and control the temperature to about 90°C. Weigh the corresponding stoichiometric amount of phosphorus oxychloride and place it in a constant pressure dropping funnel, and insert the funnel into a four-necked bottle. When the temperature of the reaction solution in the four-necked bottle is lower than 40°C, start to add phosphorus oxychloride dropwise, and control the dropping rate of phosphorus oxychloride (40-50 drops / min). Do not exceed 90°C. After the dropwise addition, the electric heating mantle was turned on to heat the reaction solution. The temperature was raised to 140°C over a period of 40 minutes, and the reaction was carried out at this temperature for 4 hours. Slowly lower the ...

Embodiment 3

[0021] Weigh 250g of octanol and pour it into a four-necked reaction flask (500ml), weigh 13.27g of sodium metal, the molar fraction of sodium alkoxide is 30%, cut the sodium into pieces and put it into the reaction flask. Start the electric stirrer, heat with an electric heating mantle, and control the temperature to about 90°C. Weigh the corresponding stoichiometric amount of phosphorus oxychloride and place it in a constant pressure dropping funnel, and insert the funnel into a four-necked bottle. When the temperature of the reaction solution in the four-necked bottle is lower than 40°C, start to add phosphorus oxychloride dropwise, and control the dropping rate of phosphorus oxychloride (40-50 drops / min). Do not exceed 90°C. After the dropwise addition, the electric heating mantle was turned on to heat the reaction solution. The temperature was raised to 130°C over a period of 40 minutes, and the reaction was carried out at this temperature for 5 hours. Slowly lower the...

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Abstract

The invention discloses a process for preparing trioctyl phosphate by a sodium alkoxide method. In the process, octanol and metal sodium react to generate sodium alkoxide, phosphorus oxychloride and the sodium alkoxide undergo esterification, and the separated product is rinsed and neutralized. The environment-friendly trioctyl phosphate synthesizing process by the sodium alkoxide method overcomes the defect that mass acid gas is generated in the conventional decompression production process so as to prevent the acid gas from polluting environment and corroding equipment. The process reduces product post-treatment difficulty, and the reclaimed octanol can be recycled, so that the raw material utilization is improved, and the production cost of the trioctyl phosphate is reduced.

Description

technical field [0001] The invention relates to a preparation process of trioctyl phosphate, which adopts an environmentally friendly sodium alkoxide method, reacts octanol (2-ethylhexanol) with metal sodium to generate sodium octanolate, and then reacts with phosphorus oxychloride (POCl 3 ) reaction to obtain trioctyl phosphate preparation technology, which belongs to the technical field of organic compound synthesis. Background technique [0002] As an important industrial raw material, trioctyl phosphate has received more and more attention. Trioctyl phosphate is mainly used in military PVC products, coatings, synthetic rubber and fibers, and can also be used in hydrogen peroxide (H 2 o 2 ) working solvents, fillers for food packaging materials, lubricating oil additives, precious metal extractants, rare earth element developer, etc. [0003] Alone from its being H 2 o 2 From the perspective of working solvent: the anthraquinone method is currently producing H 2 o 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
Inventor 张其坤
Owner SHANDONG NORMAL UNIV
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