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Monoalkyl phosphinate removal technology, product and application

A technology of alkyl phosphinate and mono-alkyl phosphinic acid, applied in application, removal process and product field of mono-alkyl phosphinate, can solve product purification, adverse environmental impact, unfavorable industrial production, etc. problems, to achieve the effect of improving the thermal stability level, strong practicability, and improving the flame retardant performance

Inactive Publication Date: 2014-08-06
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method avoids monoalkyl phosphinate, but uses two kinds of organic solvents in order to stabilize the transition metal complex, which has adverse effects on the purification of the product and the environment, and is not conducive to industrial production

Method used

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  • Monoalkyl phosphinate removal technology, product and application
  • Monoalkyl phosphinate removal technology, product and application
  • Monoalkyl phosphinate removal technology, product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Get 30g of acetic acid mixture of sodium diethylphosphinate (0.0507 mol) and sodium monoethylphosphinate (total phosphorus molar percentage is about 3.6mole%), add dropwise molar amount P-H (monoethyl sodium phosphinate) of 150mol% sodium hypochlorite aqueous solution (active chlorine content is 5.2%), reacted for 10 minutes, measured the phosphorus spectrum of the solution, and the results showed that monoethyl sodium phosphinate had been completely converted into the known ethyl phosphonic acid sodium( figure 1). Remove acetic acid and water by distillation under reduced pressure, then configure it into an aqueous solution with a concentration of 6% by mass, heat it to 90°C with stirring, slowly drop it into an aqueous solution of aluminum sulfate with a concentration of 6% by mass, and stir for 0.5h to form The white solid was filtered, the precipitate was washed with 600ml of water, and dried at 130°C for 10h to obtain aluminum diethylphosphinate (87.9% yield). Af...

Embodiment 2

[0039] Get 31.7g of an acetic acid mixture of sodium diethylphosphinate (0.0536 mol) and sodium monoethylphosphinate (total phosphorus molar percentage is about 3.6mole%), distill under reduced pressure to remove acetic acid, and add dropwise a molar amount of P-H 150mol% sodium hypochlorite solution (active chlorine content is 5.2%), reacted for 10 minutes, and measured the phosphorus spectrum of the solution. The results showed that monoethyl sodium phosphinate had all been converted into known sodium ethyl phosphonate ( figure 2 ). Then configure it into an aqueous solution with a concentration of 6% by mass, stir and heat it to 90°C, slowly drop it into an aqueous solution of aluminum sulfate with a concentration of 6% by mass, stir and react for 0.5h, a white solid is formed, filter it, and use 500ml of water The precipitate was washed and dried at 130°C for 10 h to obtain aluminum diethylphosphinate (yield 73.4%). After the product was dissolved in sodium hydroxide, th...

Embodiment 3

[0043] Nylon 66 (containing 35% glass fiber) was dried in a vacuum oven at 110°C for 4 hours, and then 70 parts (all parts by weight unless otherwise specified) were mixed with 30 parts according to Example 1 or Example 1. The aluminum diethylphosphinate prepared by the method described in 2 was mixed, and banburyed in a Brabender torque rheometer at 270° C. for 3 minutes. After drying, process it with a flat vulcanizer at 290°C to obtain a flame-retardant polymer molded product, and then use a universal sampler to cut it into a sample with a size of 100mm×13mm×3.2mm, according to the GB / T2408-2008 standard at the AG5100B level -Tested on the vertical burning tester, the result shows that it reaches the UL94 combustion level V-0.

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Abstract

The invention discloses a monoalkyl phosphinate removal technology which comprises the steps as follows: step one, an oxidizing agent is added in a mixture containing monoalkyl phosphinic acid and / or monoalkyl phosphinate and dialkyl phosphinic acid and / or dialkyl phosphinate, an oxidation reaction is finished, and a product which contains dialkyl phosphinic acid and / or dialkyl phosphinate and does not contain monoalkyl phosphinic acid and / or monoalkyl phosphinate is obtained through aftertreatment; and step two, the prepared product which contains dialkyl phosphinic acid and / or dialkyl phosphinate and does not contain monoalkyl phosphinic acid and / or monoalkyl phosphinate is subjected to a replacement reaction or a neutralization reaction to prepare dialkyl phosphinate of the salts. The invention further discloses a flame retardant prepared with the technology and an application. According to the invention, the specific oxidizing agent is adopted, monoalkyl phosphinate generates alkyl phosphonate with higher heat stability through the oxidation reaction, and the heat stability level of dialkyl phosphinate is improved, so that the flame retardant property is improved; and besides, the flame retardant can be used for various high polymer materials with fire retardance, and the flame retardant property is high.

Description

technical field [0001] The invention belongs to the field of flame retardant preparation, and in particular relates to a removal process, product and application of monoalkyl phosphinate. Background technique [0002] Aluminum and zinc dialkylphosphinates are halogen-free flame retardants with good thermal stability and flame retardancy, and have been widely used in the flame retardancy of polyamide and polyester as substitutes for brominated flame retardants. They are generally prepared by the radical-initiated addition of hypophosphorous acid or its salts to alkenes. Free radical reaction provides an economical and rapid method for obtaining dialkylphosphinates, but the dialkylphosphinates prepared by this method often contain incompletely reacted monoalkylphosphinates. [0003] For example, Chinese patent CN1284787C reports sodium hypophosphite and ethylene to prepare sodium diethylphosphinate under the action of an azo initiator, and the resulting reactant contains abou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30C08L77/06C08K5/5313C08K5/5317C08K5/3492
Inventor 姚强曹微虹
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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