A kind of method of synthesizing dimethyl methyl phosphate

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

Active Publication Date: 2021-01-05
NANTONG JIANGSHAN AGROCHEM & CHEM LIMITED LIABILITY
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  • Application Information

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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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  • A kind of method of synthesizing dimethyl methyl phosphate

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Experimental program
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Effect test

Embodiment 1

[0028]Step 1: Lewis Acid Ionic Liquid [BuPy]Cl-AlCl3(BuPy=N-butylpyridine cation) preparation:

[0029]Install a stirrer on the reaction kettle, add 26.64g (0.2mol) of anhydrous aluminum chloride under the protection of nitrogen, and add 17.1g (0.1mol) of n-butylpyridine chloride in batches. After adding the quaternary ammonium salt, keep it at 60℃ and stir for 3 hours to ensure the reaction is complete, and a transparent light brown [BuPy]Cl-AlCl is obtained.3Ionic liquid.

[0030]Step 2: Preparation of dimethyl methyl phosphate

[0031](1) Install a stirrer on the reactor, and equip it with a cold circulation cooling system to ensure reflux, put in the above ionic liquid, 124g (1mol) of trimethyl phosphite and heat to reflux, then heat to 80℃-100℃, and the pressure is controlled at 1.1 -Between 2.1 atmospheres, after 6 hours of reaction, GC detects that the conversion rate of raw materials is 99%.

[0032](2) Collect the reaction liquid, stand still for layering, obtain 110.12 g of the target...

Embodiment 2

[0038]The first step: ionic liquid [Et3NH]Cl-AlCl3(Et3NH = hydrogenated triethylamine cation) preparation:

[0039]Install a stirrer on the reaction kettle, add 26.64g (0.2mol) of anhydrous aluminum chloride under the protection of nitrogen, and add 13.8g (0.1mol) of triethylamine hydrochloride in batches. After adding the quaternary ammonium salt, keep it at about 120℃ and stir for 2h to ensure the reaction is complete, and the obtained transparent and colorless [Et3NH]Cl-AlCl3Ionic liquid.

[0040]Step 2: Preparation of dimethyl methyl phosphate

[0041](1) Install a stirrer on the reactor and equip it with a cold circulation cooling system to ensure reflux. Put in the above ionic liquid, 124g (1mol) of trimethyl phosphite and heat to reflux, then heat to 80℃-100℃, and control the pressure at 1.2 -Between 1.5 atmospheres, after 4 hours of reaction, the conversion rate of raw materials is 99.5% detected by GC.

[0042](2) Collect the reaction liquid, stand still for layering, obtain 116.02g of...

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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 internationally. It is suitable for flame retardant additives in polyurethane products, unsaturated polyester resins and epoxy resins and other polymer materials, or as dye additives, metal extractants, Heat stabilizer, plant growth regulator, etc.[0003]There are three main methods for synthesizing flame retardant DMMP:[0004](1) DMMP is generated by the reaction of dimethyl phosphate under the catalyst, the reaction formula is as follows:;[0005]However, this reaction uses highly toxic cyanide as a catalyst, which is not only unfavorable for operation, but also difficult to purify the product. (2) Thermal cracking method generates DMMP, the...

Claims

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Application Information

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