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Method for preparing fluorine-containing phosphate ester surfactant

A technology of surfactants and fluorine-containing phosphate esters, applied in chemical instruments and methods, transportation and packaging, dissolution, etc., can solve problems such as darkening of product color, excessive local reaction, carbonization, etc. Effect of improving product quality and suppressing darkening of color

Inactive Publication Date: 2015-11-25
焦作超达环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of adding phosphorylation reagents at one time or in batches, it is difficult to disperse uniformly in time, resulting in too fast local reaction, and it is difficult to control the ratio of mono- and di-esters in the product.
In addition, if the heat of reaction cannot be taken away in time, the color of the product will become darker, or even partially carbonized, which will affect the quality and use of the product.
In order to obtain high-quality phosphate esters, it is usually necessary to purify the product and separate mono- and di-esters, and the process is complex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Prepare 895g of perfluoroalkoxylated fluorinated polyether (molecular weight: 600) into a 60% mass concentration toluene solution. 95gH 3 PO 4 Polyphosphoric acid with a content of 105% is made into a toluene solution with a mass concentration of 60%. 50 g of toluene was added into the reaction kettle, and the temperature was raised to 40°C. At the same time, add the prepared fluorine-containing polyether toluene solution and polyphosphate toluene solution dropwise, keep the feeding speed uniform, and finish dropping in 2 hours. During the dropwise addition, the temperature of the reactor was controlled not to exceed 60°C. After dropping, the temperature was raised to 80° C., and aged for 2 hours. Toluene was removed under reduced pressure to obtain 1000 g of fluorophosphate ester surfactant.

[0021] According to potentiometric titration analysis, the composition of the fluorine-containing phosphoric acid ester surfactant is as follows: the content of monoester is...

Embodiment 2

[0023] 880g of partially fluorinated alkoxylated fluorine-containing polyether (molecular weight: 540) was formulated into a toluene solution with a mass concentration of 80%. 93gH 3 PO 4 Polyphosphoric acid with a content of 110% is made into a toluene solution with a mass concentration of 80%. 197g of toluene was added into the reaction kettle, and the temperature was raised to 40°C. At the same time, add the prepared fluorine-containing polyether solution and polyphosphoric acid solution dropwise, keep the feeding speed uniform, and finish dropping in 3 hours. During the dropwise addition, the temperature of the reactor was controlled not to exceed 60°C. After dropping, the temperature was raised to 80° C., and aged for 3 hours. After removal of toluene under reduced pressure, 983 g of fluorophosphate ester surfactant was obtained.

[0024] Through potentiometric titration analysis, the composition of the fluorine-containing phosphate ester surfactant is: monoester con...

Embodiment 3

[0026] 830g of partially fluorinated alkoxylated fluorine-containing polyether (molecular weight: 583) was made into a 90% mass concentration toluene solution. 88gH 3 PO 4 Polyphosphoric acid with a content of 120% is made into a toluene solution with a mass concentration of 90%. 93g of toluene was added into the reaction kettle, and the temperature was raised to 40°C. At the same time, drop the prepared fluorine-containing polyether solution and polyphosphoric acid solution, keep the feeding speed uniform, and finish dropping in 4 hours. During the dropwise addition, the temperature of the reactor was controlled not to exceed 60°C. After dropping, the temperature was raised to 80° C., and aged for 4 hours. After removal of toluene under reduced pressure, 927 g of fluorophosphate ester surfactant was obtained.

[0027] According to the potentiometric titration analysis, the composition of the fluorine-containing phosphoric acid ester surfactant is as follows: the content ...

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Abstract

The invention discloses a method for preparing a fluorine-containing phosphate ester surfactant. The method particularly comprises the following steps: preparing a fluorine-containing polyether toluene solution and a poly-phosphate toluene solution separately; adding toluene into a reaction kettle, and heating to 40 DEG C; continuously dripping the fluorine-containing polyether toluene solution and the poly-phosphate toluene solution into the reaction kettle with an uniform speed, and performing an esterification reaction for 2-4 hours when the reaction temperature is controlled to be 60 DEG C or below; heating to 80 DEG C, and curing for 2-4 hours; removing toluene under reduced pressure to obtain the fluorine-containing phosphate ester product. By adjusting a feeding mode, the reactants are continuously added with the uniform speed in the reaction process, so that the esterification reaction process is effectively controlled, the ratio of monoester to diesters in the product can be controlled, the color of the product is prevented from being darker, and the product quality is improved.

Description

technical field [0001] The invention provides a method for preparing a fluorine-containing phosphate surfactant, and belongs to the technical field of surfactant preparation. Background technique [0002] Fluorine-containing phosphate is a kind of surfactant with excellent performance, which can significantly reduce the surface tension of aqueous solution, acid and alkali resistance, high temperature resistance, and has incomparable advantages over ordinary surfactants. It is widely used in many fields such as medicine, chemical industry and pesticide. [0003] Fluorine-containing phosphates are usually prepared by reacting fluorine-containing compounds with phosphorylation reagents. Commonly used phosphorylation reagents include phosphorus oxychloride, phosphorus pentoxide, phosphoric acid and polyphosphoric acid. The commonly used synthesis method is to put the fluorine-containing compound into the bottom of the kettle, and add the phosphorylation reagent into the reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/14C08G65/00C09K23/14
Inventor 宋学娟郝立国
Owner 焦作超达环保科技有限公司
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