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Method for synthesizing dimethyl methylphosphate

A technology of dimethyl methyl phosphate and trimethyl phosphite, which is applied in the field of synthesis of alkyl phosphate compounds, can solve the problem of low reaction yield and achieve the effects of high product purity, convenient operation and mild reaction conditions

Active Publication Date: 2018-03-13
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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Problems solved by technology

Under the protection of an inert gas, the raw material trimethyl phosphite was mixed and stirred with an appropriate amount of benzenesulfonic acid catalyst, and the target product dimethyl phosphate was synthesized by a rearrangement reaction through pressurized heating, but the reaction yield was not high, only Can reach about 93%

Method used

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  • Method for synthesizing dimethyl methylphosphate

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Effect test

Embodiment 1

[0029] Step 1: Lewis Acid Ionic Liquid [BuPy]Cl-AlCl 3 Preparation of (BuPy=N-butylpyridinium cation):

[0030] Install a stirrer on the reaction kettle, add 26.64g (0.2mol) of anhydrous aluminum chloride under nitrogen protection, and add 17.1g (0.1mol) of n-butylpyridine chloride in batches. After adding the quaternary ammonium salt, keep stirring at about 60°C for 3 hours to ensure the reaction is complete, and a transparent light brown [BuPy]Cl-AlCl is obtained 3 ionic liquid.

[0031] The second step: the preparation of dimethyl methyl phosphate

[0032] (1) Install a stirrer on the reaction kettle, and equip it with a cold circulation cooling system to ensure reflux. Put in the above-mentioned ionic liquid and 124g (1mol) trimethyl phosphite to heat and reflux, then raise the temperature to 80°C-100°C, and control the pressure at 1.1 - Between 2.1 atmospheric pressure, after reacting for 6 hours, the conversion rate of raw materials detected by GC was 99%.

[0033] (...

Embodiment 2

[0039] Step 1: Ionic liquid [Et 3 NH]Cl-AlCl 3 (Et 3 Preparation of NH = hydrogenated triethylamine cation):

[0040] Install a stirrer on the reaction kettle, add 26.64g (0.2mol) of anhydrous aluminum chloride under nitrogen protection, and add 13.8g (0.1mol) of triethylamine hydrochloride in batches. After adding the quaternary ammonium salt, keep stirring at about 120°C for 2 hours to ensure that the reaction is complete, and a transparent and colorless [Et 3 NH]Cl-AlCl 3 ionic liquid.

[0041] The second step: the preparation of dimethyl methyl phosphate

[0042] (1) Install a stirrer on the reaction kettle, and equip it with a cold circulation cooling system to ensure reflux. Put in the above-mentioned ionic liquid and 124g (1mol) trimethyl phosphite to heat and reflux, then raise the temperature to 80°C-100°C, and control the pressure at 1.2 - Between 1.5 atmospheric pressure, after reacting for 4 hours, the conversion rate of raw materials detected by GC was 99.5%...

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Abstract

The invention provides a method for synthesizing dimethyl methylphosphate. The method comprises the following synthesizing steps: synthesizing lewis acid ionic liquid, namely, mixing quaternary ammonium salt and anhydrous aluminium chloride based on the molar ratio of 1:(1-4), and heating to obtain the ewis acid ionic liquid; mixing, heating and pressurizing trimethyl phosphite and the ionic liquid obtained in step 1; decreasing the temperature of the mixture after the reaction; allowing standing still for layering to obtain a lower ionic liquid mixing and dissolving layer and an upper dimethyl methylphosphate product layer. According to the method, little lewis acid ionic liquid is used; the activity of a catalyst remains in the reaction and separating process; the synthesized product ishigh in purity.

Description

technical field [0001] The invention relates to a synthesis technology of an alkyl phosphate compound. Background technique [0002] Materials used in construction, transportation, aviation, electrical appliances, household furniture and other industries often require flame retardant properties. DMMP is a phosphorus-containing flame retardant widely used in the world. It is suitable for flame retardant additives of polymer materials such as polyurethane products, unsaturated polyester resins and epoxy resins, or as a dye auxiliary, metal extractant, Heat stabilizers, plant growth regulators, etc. [0003] There are three main ways to synthesize flame retardant DMMP: [0004] (1) DMMP is generated by the reaction of dimethyl phosphate under the catalyst, and the reaction formula is as follows: [0005] ; [0006] However, what this reaction uses is highly toxic cyanide as a catalyst, which is not only unfavorable for operation, but also the product is difficult to purif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40
CPCC07F9/4075
Inventor 黄波刘晨晨沈康吉伟崔剑
Owner NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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