Process for producing alkyl phosphonic acid

A technology for alkane phosphonic acid and alkane phosphonic acid ester, which is applied in the field of preparing alkane phosphonic acid, can solve the problems of low product purity, difficult separation and purification, and many by-products, and achieves simple process flow, high purity, and high yield. rate stabilization effect

Active Publication Date: 2009-05-13
SINOMAX SOLUTIONS CO LTD
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  • Abstract
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Problems solved by technology

Patent (US6420598) has reported a kind of propylphosphoric acid synthetic method under high pressure, and this method is with phosphorous acid and propylene gas as raw material, synthesizes propylphosphoric acid under 4Mpa pressure, because alkene addition easily occurs rearrangement in the reaction process, so by-product There are many products, the product purity is not high, the main content is about 80%, and it is difficult to separate and purify

Method used

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  • Process for producing alkyl phosphonic acid

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Embodiment 1

[0021] Embodiment 1: Lithium 175g (25mol) is joined in the 30L toluene of 110 ℃, reflux sanding, dropwise add methyl propyl phosphite 3.46kg (25mol), continue to stir and reflux for 6 hours, dropwise add chloroethane 1.94kg ( 30mol), reflux reaction for 18 hours, lowering the temperature, filtering and reclaiming a little lithium remaining, the filtrate first reclaims toluene under normal pressure, then distills under reduced pressure to obtain methylpropyl ethylphosphonate, adds glacial acetic acid to methylpropyl ethylphosphonate, Hydrolyze until the reaction is complete, dehydrate to obtain the crude product, and recrystallize from toluene to obtain 1782 g of white flaky solid ethylphosphonic acid with a yield of 64.8% and a purity of 96.3%.

Embodiment 2

[0022] Example 2: Add 575 g (25 mol) of sodium to 32 L of xylene at 145 ° C, reflux to sand, add 2.76 kg (25 mol) of dimethyl phosphite dropwise, continue to stir and reflux for 12 hours, and add 3.27 kg of bromoethane dropwise (30mol), reflux reaction for 18 hours, lower the temperature, filter and recover a little residual sodium, the filtrate first recovers xylene under normal pressure, then distill under reduced pressure to obtain dimethyl ethylphosphonate, add hydrogen to dimethyl ethylphosphonate Sodium oxide was hydrolyzed until the reaction was complete, and the crude product was obtained by dehydration, which was recrystallized from toluene to obtain 1869 g of white flaky solid ethylphosphonic acid with a yield of 67.9% and a purity of 95.6%.

Embodiment 3

[0023] Example 3: Add 978g (25mol) of potassium to 30L of toluene at 130°C, reflux to sand, add 3.46kg (25mol) of methyl propyl phosphite dropwise, continue to stir and reflux for 6 hours, and add 2.36kg of 1-chloropropane dropwise (30mol), reflux reaction for 18 hours, lower the temperature, filter and recover a little lithium remaining, the filtrate first recovers toluene under normal pressure, then distills under reduced pressure to obtain methylpropyl ethylphosphonate, and adds glacial acetic acid to methylpropyl ethylphosphonate , hydrolyzed until the reaction was complete, and dehydrated to obtain a crude product, which was recrystallized from toluene to obtain 2010 g of white flaky solid propylphosphonic acid with a yield of 64.8% and a purity of 96.3%.

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Abstract

The invention relates to a method for preparing alkyl phosphonic acid, which comprises the following steps: (1) an alkali metal reacts with phosphite ester to obtain phosphite ester; (2) the phosphate ester reacts with halogenated alkane to obtain alkyl phosphonate ester; and (3) the alkyl phosphonate ester is hydrolyzed to obtain the alkyl phosphonic acid. The method has the advantages of reasonable reaction steps which are carried out at normal pressure, mild and smooth process condition, simple process flow, higher purity of obtained products, comparatively stable yield, and better industrialized prospect, and can be used for preparing various alkyl phosphonic acids, such as methylphosphoric acid, ethylphosphonic acid, propylphosphonic acid and the like.

Description

technical field [0001] The present invention relates to a process for the preparation of alkylphosphonic acids. Background technique [0002] Alkyl phosphonic acid is an important organic acid. It is widely used in water softening, flotation beneficiation, fireproof materials, pesticides and other fields by itself or its salt, ester and anhydride. Recently, it is also used as an irreversible dehydrating agent in The development abroad is very rapid. [0003] Griffin (J.Org.Chem., 24, 2049, 1959) reported a method for the synthesis of alkane-based phosphonic acid, which uses phosphorous acid and olefins as raw materials, and uses glacial acetic acid or dioxane as a solvent to prepare alkane-based phosphoric acid , because what adopt is free radical reaction, the by-product of this method is many, and yield is between 18-28%. Patent (US6420598) has reported a kind of propylphosphoric acid synthetic method under high pressure, and this method is with phosphorous acid and prop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 高建勋周东董洪荣
Owner SINOMAX SOLUTIONS CO LTD
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