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Method for manufacturing alkyl-phosphates

A technology of tetraalkyl diphosphate and tetrachlorodiphosphate, which is applied in the field of preparation of tetraalkyl diphosphate, can solve the problems of being unsuitable for industrial production, impurity prevention or removal, expensive, moderate, etc.

Inactive Publication Date: 2012-07-25
LANXESS DEUTDCHLAND GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, they have the disadvantage that the prevention or removal of the aforementioned impurities is expensive and inconvenient, and thus unsuitable for industrial production
[0008] Furthermore, the disadvantages of this method are the only moderate yields and the fact that the method involves multiple liquid-liquid phase separations
Therefore, this method is poorly suitable for the preparation of partially water-soluble tetraalkyl diphosphates and is not at all suitable for the preparation of completely water-soluble tetraalkyl diphosphates

Method used

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  • Method for manufacturing alkyl-phosphates

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0099] Example 1: Preparation of diethylene glycol bis(dichlorophosphate) (not of the invention)

[0100] Into a 1,000 ml four-neck flask with stirrer, thermometer, dropping funnel (with pressure compensation) and reflux condenser was added 984.3 g of phosphorus oxychloride at 20°C. A vacuum of approximately 670 mbar was then applied and 332.3 g of diethylene glycol were added dropwise within 4 hours. Cool in an ice-water bath, keeping the temperature at 20 °C. A clear, colorless reaction mixture formed. At the end of the metered addition, the pressure was reduced to about 6 mbar and stirring was continued at 25° C. for 16 hours. This left 1055.7 g (98%) of diethylene glycol bis(dichlorophosphate).

example 2

[0101] Example 2: Preparation of tetraethyldiethylene glycol diphosphate (of the present invention)

[0102] Into a 1000 ml four-necked flask with stirrer, thermometer, dropping funnel (with pressure compensation) and reflux condenser under nitrogen atmosphere was added 169.8 g of diethylene glycol bis(dichlorophosphate) from Example 1, and The initial charge was cooled to 10 °C. At this temperature, 350 ml of ethanol were added dropwise within 50 minutes. Dry ice pellets were dropped in to maintain the temperature at 10°C-15°C. The colorless solution was then stirred at 15°C for 1 hour and then at 23°C for 2 hours. The colorless, clear synthesis solution was then mixed dropwise within 2 hours with a mixture of 340 ml of water and 155 g of a 50% strength sodium hydroxide solution. Cool in an ice-water bath, keeping the temperature at 20 °C. The mixture was then stirred at 23° C. for 16 hours and extracted with four times 100 ml of dichloromethane. The combined extract s...

example 3

[0105] Example 3: Preparation of tetraethyldiethylene glycol diphosphate (of the present invention)

[0106]Into a 1000 ml four-necked flask was added 169.8 g of diethylene glycol bis(dichlorophosphate) from Example 1 at 5°C under nitrogen. At this temperature, 276.4 g of ethanol were added dropwise within 50 minutes. The reaction mixture showed an exothermic reaction. An ice-water bath was used to maintain the temperature of the reaction mixture at 10°C. The clear, slightly orange-brown solution was then stirred at 10° C. for 2 hours, then warmed to 20° C. and stirred for a further 18 hours. Into a 2 liter glass beaker was added 340 ml of completely demineralized water, followed by the addition of 155 g of 50% strength sodium hydroxide solution with stirring. The mixture was cooled to 23°C. The above synthesis solution was then metered in over 2 hours, with the formation of a slight mist. The temperature was maintained at 23°C by external cooling. The yellowish mixtur...

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Abstract

Preparing fully or partially water-soluble tetraalkylbisphosphates (I) comprises: (a) reacting tetrachlorbisphosphates (II) with one or more different alcohols; (b) reacting the reaction mixture of step (a) with a base; (c) adding water to the reaction mixture of step (b); (d) adding solvent that is not completely miscible with water to the reaction mixture of step (c) to form a mixture consisting of two separate liquid phases; and (e) separating a phase containing (I) that is obtained in step (d). Preparing fully or partially water-soluble tetraalkylbisphosphates (I) comprises: (a) reacting tetrachlorbisphosphates (II) with one or more different alcohols; (b) reacting the reaction mixture of step (a) with a base containing one or more substance of formula ((Kat(n+)) a(X(m-)) b), when at least 50% of (II) containing phosphorus-chloride groups are reacted; (c) adding water to the reaction mixture of step (b); (d) adding solvent that is not completely miscible with water to the reaction mixture of step (c) to form a mixture consisting of two separate liquid phases; and (e) separating a phase containing (I) that is obtained in step (d).

Description

technical field [0001] The present invention relates to a process for the preparation of tetraalkyl diphosphates by reacting tetrachlorobisphosphates with alcohols, neutralizing the resulting hydrogen chloride with a base, and separating it from the reaction mixture by extraction produce the desired product. Background technique [0002] Tetraalkyl diphosphates are low volatility viscous liquids and have been used for a long time in industrial applications, eg as polymer additives (see US 2,782,128) or as hydraulic oils (see US 4,056,480). For these applications, it is typically necessary that the tetraalkyl diphosphates contain as few impurities as possible. Therefore, the amount of acidic impurities, which may be determined, for example by measuring the acid number, should be very low, since acids may lead to accelerated decomposition or corrosion. Tetraalkyl diphosphates with acid numbers greater than about 1.0 mg KOH / g are not useful in the enumerated applications. As...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
CPCC07F9/091C07F9/14C07F9/093F24F7/013F24F11/30F24F13/20F24F13/28F24F2110/20F24F2110/50
Inventor 扬-格尔德·汉塞尔
Owner LANXESS DEUTDCHLAND GMBH
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