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Synthetic method for phosphate ester

A synthesis method and phosphate ester technology, which are applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of large differences in the ratio of mono- and di-esters of phosphate esters and uneven reaction systems , severe local reaction, etc., to achieve good reproducibility, avoid coking and carbonization, and mild reaction

Inactive Publication Date: 2014-06-04
SOUTH CHINA NORMAL UNIVERSITY +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the existing phosphorus pentoxide type is usually synthesized by a solvent-free method. This method has some disadvantages, mainly the problem of uneven reaction system and excessive local reaction, which easily leads to a large amount of coking and carbonization of phosphate ester, and the yield is usually Only 50-60%; under the same conditions, the proportion of mono- and di-esters of phosphate esters synthesized by different batches varies greatly, and the reproducibility is poor

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  • Synthetic method for phosphate ester

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Effect test

Embodiment 1-11

[0018] The reactants and organic solvents in Examples 1-11 are all the same, 0.1 mol of phosphorus pentoxide, 0.2 mol of n-octanol and 100 mL of toluene.

[0019] The preparation method is as follows:

[0020] Mixing: Put phosphorus pentoxide in a beaker, add toluene to the beaker, and stir with a magnetic stirrer to fully disperse phosphorus pentoxide; then divide n-octanol into four parts and add them to the beaker (Example 11, n-octanol was added to the beaker all at once), the interval between the addition of two parts of n-octanol was 10 minutes, and after stirring for 15 minutes, the solution in the beaker changed from milky white to clear.

[0021] Esterification: Transfer the solution in the beaker to a 250mL two-necked bottle and place the two-necked bottle in an oil bath, heat the oil bath to a certain temperature, and maintain this temperature for a period of time.

[0022] Hydrolysis: Add deionized water into the two-necked bottle, and then heat the oil bath to a ...

Embodiment 12-21

[0027] The preparation method of phosphoric acid ester in embodiment 12-21 is as follows:

[0028] Mixing: Put phosphorus pentoxide in a beaker, add 100mL organic solvent into the beaker, stir with a magnetic stirrer to fully disperse phosphorus pentoxide; then divide the primary alcohol into four parts and add them to the beaker one by one, two The interval time of part of primary alcohol adding is 10min, and after continuing to stir for 15min, the solution in the beaker becomes clear by milky white.

[0029] Esterification: Transfer the solution in the beaker to a 250mL two-necked bottle and place the two-necked bottle in an oil bath, heat the oil bath to 65°C (75°C in Example 20-21), and maintain this temperature for 3h ( The reaction time of Examples 19-21 is 3.5h).

[0030] Hydrolysis: add 10 mL of deionized water to the two-necked bottle (the deionized water in Example 19-21 is 5 mL), then heat the oil bath to 75°C (85°C in Example 20-21), and hydrolyze for 1 hour.

[...

Embodiment 22

[0041] Taking Example 4 as a reference, the reaction was amplified 100 times, that is, 10mol, 1.42Kg of phosphorus pentoxide and 20mol, 2.6046kg of n-octanol were reacted.

[0042] Mixing: Put phosphorus pentoxide in a container, add 10L organic solvent into the container, stir with a stirrer to fully disperse phosphorus pentoxide; then divide n-octanol into four parts and add them to the container one by one, The interval between the addition of two parts of n-octanol is 10 minutes, and after stirring for 15 minutes, the solution in the container changes from milky white to clear.

[0043] Esterification: Transfer the solution in the container to a double-ported reaction tank and heat the reaction tank to 65°C, maintaining this temperature for 3 hours.

[0044] Hydrolysis: Add 1L of deionized water to the reaction tank, then continue heating to raise the temperature of the reaction tank to 75°C, and hydrolyze for 1 hour.

[0045] Separation: Stop heating the reaction tank af...

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Abstract

The invention relates to the technical field of chemical synthesis, and particularly relates to a synthetic method for phosphate ester. The synthetic method comprises the steps of subjecting phosphorus pentoxide and primary alcohol to an esterification reaction in an organic solvent; and then hydrolyzing and extracting to obtain the phosphate ester. The phosphate ester is prepared by a phosphorus pentoxide solvent method. The reaction is mild, so that the problem of non-uniform reaction system and too vigorous local reaction can be effectively prevented, thereby preventing coking and carbonization phenomena of the phosphate ester. Besides, by controlling reaction conditions, particularly a reaction solvent, a reaction temperature and a reaction time, a proportion of monoester to diester in a product can be controlled; repeatability is good; the content of monoester in the product is 48-52%; and the method is suitable for preparing excellent rust-preventative oil. By controlling a hydrolysis time, a hydrolysis temperature and water use amount and by using diethyl ether as an extracting agent, reaction yield can be obviously increased; and yield can reach as high as 80-90%. Besides, control of a feeding manner of the primary alcohol can also increase the yield and influence the proportion of the monoester to the diester.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for synthesizing phosphoric acid esters. Background technique [0002] Phosphate esters are produced by esterification of hydroxyl-containing organic compounds with phosphating agents. Since phosphoric acid is a tribasic acid, according to the number of substituted hydrocarbon groups, phosphoric acid esters can be divided into primary phosphoric acid esters (monophosphoric acid esters, hydrocarbyl phosphoric acid esters), secondary phosphoric acid esters (phosphoric acid diesters) and tertiary phosphoric acid esters (phosphoric acid triesters). . There are many existing methods for synthesizing phosphate esters. According to different phosphating agents, they can be divided into phosphorus pentoxide type, phosphorus trihalide type, phosphorus oxyhalide type, phosphoric acid type and pyrophosphoric acid type, etc., but most of them are only suitable for Carry...

Claims

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Application Information

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IPC IPC(8): C07F9/11C23F11/167
Inventor 蒋腊生张培唐陆赵淑婷黄伟聪黎汉超欧博明
Owner SOUTH CHINA NORMAL UNIVERSITY
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