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Preparation method and application of diethyl phosphinates

A technology of diethylphosphinate and hypophosphorous acid, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of reducing the safety of the reaction system and increasing the cost of product synthesis , high energy consumption and other issues, to achieve the effect of lowering the temperature, inhibiting the formation of by-products, and lowering the reaction temperature

Inactive Publication Date: 2010-11-24
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

, therefore, the temperature required for the reaction system is higher, and its energy consumption is larger, which increases the synthesis cost of the product
In addition, most of the commonly used reaction solvents are low-boiling substances, while the decomposition temperature of peroxide catalysts exceeds 100 °C
In order to make the reaction go smoothly, pressurization is generally used to increase the boiling point of the solvent system, which greatly reduces the safety of the reaction system.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 106g (1mol) sodium hypophosphite monohydrate in 750ml water, then move the solution to a 2L jacketed pressure-resistant reactor equipped with a UV lamp, keep the temperature of the reaction solution at room temperature, and then pass through ethylene gas , the pressure in the kettle is maintained at 5atm, and reaches saturation, then the ultraviolet lamp is energized, and the ultraviolet light irradiates the reaction solution, and 1.45g (2.5mol%) of acetone is uniformly and slowly dripped in 6 hours simultaneously, and the photoinitiator is dripped After completion, the reaction was continued for 1 hour, the reactor was depressurized, and the resulting solution was heated to 90°C. Slowly drop aluminum chloride solution (42.5g (0.35mol) dissolved in 100g water) and add it within 60min. The resulting suspension was filtered to give a white solid, which was washed with 1 L of hot water and dried under vacuum at 130°C. The resulting solid was analyzed.

[0029] ...

Embodiment 2

[0034] Dissolve 106g (1mol) of sodium hypophosphite monohydrate in 400ml of acetic acid, then move the solution to a 2L jacketed pressure-resistant reactor equipped with a UV lamp, then maintain the temperature of the reaction solution at room temperature, and then pass through ethylene gas to keep the pressure in the kettle at 6atm and reach saturation, then the UV lamp is energized, and the UV light irradiates the reaction solution, and at the same time, 2.2g (5mol%) acetaldehyde is uniformly and slowly dripped in within 8 hours, until it is completely dripped Afterwards, the reaction was performed for another 1 hour, the reactor was depressurized, and the resulting solution was heated to 85°C. Slowly drop aluminum acetate solution (81.9g (0.35mol) dissolved in 150g water) and add it within 60min. The resulting suspension was filtered to give a white solid, which was washed with 1 L of hot water and then dried under vacuum at 130°C. The resulting solid was analyzed.

[003...

Embodiment 3

[0040] Obtain the sodium diethylphosphinate solution according to Example 1, and then heat the solution to 85°C. Slowly drop aluminum sulfate solution (233.1gAl 2 (SO 4 )3·18H 2 O (0.35 mol) dissolved in 150 g of water), was added within 60 min and the resulting suspension was filtered to obtain a white solid, which was washed with 1 L of hot water and then dried under vacuum at 130°C. The resulting solid was analyzed.

[0041] 31 P NMR

[0042] Aluminum diethylphosphinate: 84.7%

[0043] Aluminum monoethylphosphinate: 4.1%

[0044] Unidentified compounds: 11.2%.

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PUM

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Abstract

The invention discloses a preparation method and application of diethyl phosphinates, belonging to the field of green flame retardants. The preparation method of the diethyl phosphinates comprises the following steps of: making hypophosphorous acid and / or an alkali metal salt thereof react with ethylene under the irradiation of ultraviolet light in the presence of a photoinitiator in a solvent system to obtain diethyl phosphinic acid and / or an alkali metal salt thereof; and making the obtained diethyl phosphinic acid and / or the alkali metal salt thereof react with metallic compounds of Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Ce, Sn and / or Fe to obtain corresponding diethyl phosphinates. In the invention, the photoinitiator is decomposed into free radicals under the irradiation of the ultraviolet light to initiate an additive reaction so that the reaction rate can be improved, the energy consumption required in the reaction can be reduced and the production cost of products can be lowered.

Description

Technical field: [0001] The invention belongs to the field of green and environment-friendly flame retardants, and relates to a preparation method and application of diethylphosphinate. Background technique: [0002] At present, organophosphorus compounds are increasingly showing their importance in industrial production. They can be used to prepare pesticides, extractants and flame retardants, etc. Among them, salts of organic phosphonic acids are widely used as flame retardants, and there are many types of preparation methods. [0003] For example, US 6011172 and CN1280581 describe the preparation of alkylphosphinic acids and dialkylphosphinates from elemental yellow phosphorus and alkyl halides in the presence of aqueous alkali metal hydroxide or alkaline earth metal hydroxide solutions The organic solvent system is also used in the reaction, and the obtained product belongs to the mixed system in which the alkylphosphonous acid is the main component. The disadvantage o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C09K21/12
Inventor 张宝贵杨丽韩新宇毕良成周逸潇唐雪娇
Owner NANKAI UNIV
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