Preparation method of high-purity dioctyl phosphate

A dioctyl phosphate and high-purity technology, applied in the field of preparing high-purity dioctyl phosphate, can solve the problems of long production cycle and high production energy consumption, and achieve the effects of short reaction cycle, improved purity and reduced dosage

Pending Publication Date: 2021-11-30
HANGZHOU QIANYANG TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of high-purity phosphoric acid in order to solve the defects that the production energy consumption of di-isooctyl phosphate prepared from existing tri-iso-octyl phosphate is high, the production cycle is long, and the content meter yield is lower than 90%. The preparation method of dioctyl phosphate, the present invention utilizes the by-product produced in the production process of trioctyl phosphate to prepare high-purity dioctyl phosphate, does not need to add phase transfer catalyst, the steps are simple, the reaction conditions are mild, the energy consumption is low, and the reaction cycle is shorter Short, the content of dioctyl phosphate obtained is greater than 93%, and the purity is high

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  • Preparation method of high-purity dioctyl phosphate
  • Preparation method of high-purity dioctyl phosphate

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Experimental program
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Embodiment

[0027] Add 100g of mixed octyl phosphates into a 250mL three-necked flask equipped with a stirring rod (wherein, the mass fraction of dioctyl phosphate is 66-68%, the mass fraction of monooctyl phosphate is 2-4%, and the mass fraction of trioctyl phosphate The mass fraction is 30~33%, and this mixed octyl phosphate comes from the by-product produced in the production process of trioctyl phosphate), 10g water, 30g octanol, carry out reaction at 120~130 ℃ for 6 hours, after the reaction finishes, go to Slowly add 100g of normal temperature water into the material, then acidify with concentrated hydrochloric acid until the pH value reaches 2-7, stir for 10-20 minutes, separate the layers after standing still, and separate the water phase. Then wash with 100g of water at 60-70°C for 3 times, then add 40-50g of hot water at 60-70°C and acidify with concentrated hydrochloric acid until the pH value is less than 1, stir for 10-20 minutes, separate the water phase, and then the organic...

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Abstract

The invention provides a preparation method of high-purity dioctyl phosphate, which comprises the following steps: taking octanol and water as solvents, adding phosphoric acid mixed octyl ester and solid alkali which is 1.1-1.35 times of theoretical quantity required by alkaline hydrolysis of the phosphoric acid mixed octyl ester, performing high-temperature alkaline hydrolysis, and performing acidification reaction twice to obtain the high-content and high-purity dioctyl phosphate. According to the method, the dosage of the solid alkali is reduced, a phase transfer catalyst does not need to be added, the steps are simple, the reaction conditions are mild, the energy consumption is low, the reaction period is short, the content of the obtained dioctyl phosphate is larger than 93%, and the purity is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a method for preparing dioctyl phosphate, in particular to a method for preparing high-purity dioctyl phosphate by using by-products produced in the production process of trioctyl phosphate. Background technique [0002] Dioctyl phosphate, also known as p204, Chinese name: bis(2-ethylhexyl) phosphate; bis(2-ethylhexyl) phosphate; diisooctyl phosphate; dioctyl phosphate, national CAS registration number: 298-07-7 is a colorless, transparent and viscous liquid. Freezing point -60°C, relative density 0.973 (25 / 25°C), refractive index 1.4420 (25°C), boiling point 209°C (1.33kPa). Product application: used as an organic solvent, an acidic extractant, and an intermediate in organic synthesis. In kerosene, it exists as a hydrogen-bonded dimer structure to cover its polar phosphate groups, and usually participates in the reaction in dimerization when it complexes with metal ion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
CPCC07F9/11
Inventor 黄阳卫李守勤骆益鸣陈勤勇边江
Owner HANGZHOU QIANYANG TECH
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