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Synthesis process of phosphinate containing alkylaryl

A technology of alkylaryl phosphinate and alkylaryl phosphonate, which is applied in the field of synthesis of organic phosphinate flame retardants, can solve problems such as reducing reaction efficiency, and achieve abundant raw material sources and excellent reaction conditions Gentle, easy-to-use effect

Inactive Publication Date: 2015-03-25
NANJING JINYUAN FLAME RETARDANT TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the reaction uses olefins as raw materials, it needs to be reacted under high pressure; at the same time, because the free radical initiator is easy to cause the polymerization of olefins themselves, the actual reaction efficiency is reduced.
[0004] The present invention aims to overcome the deficiencies in the synthesis process of organic phosphinate flame retardants in the prior art, and provides a new process for the synthesis of phosphinates containing aryl and alkyl groups in their molecular structure

Method used

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  • Synthesis process of phosphinate containing alkylaryl
  • Synthesis process of phosphinate containing alkylaryl
  • Synthesis process of phosphinate containing alkylaryl

Examples

Experimental program
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Embodiment 1

[0037] The synthesis of embodiment 1 aluminum ethyl phenyl phosphinate

[0038] The first step: the synthesis of diethyl phenylphosphonite

[0039] Add 27.6g of ethanol, 22.2g of triethylamine and 100ml of chloroform into a flask equipped with a stirring, condensing, and drying device, start stirring, cool to 0°C in an ice-water bath, and slowly add 35.9 The chloroform solution of g phenylphosphorus dichloride was dropped in about 2 hours; keep at 0-10°C, monitor the reaction by PNMR, and stop the reaction after about 3 hours. After the reaction was completed, the generated solid was filtered off, the solvent and excess ethanol were removed by spin (steaming), and the obtained product was purified by distillation under reduced pressure, and a fraction at 107-109°C / 12mmHg was cut off. By weighing, 32.5 g of the product was obtained, and the product yield was 82.1%.

[0040] The second step: the synthesis of phenyl ethyl phosphonate

[0041] Put 32.3 g of diethyl phenylphosph...

Embodiment 2

[0044] The synthesis of embodiment 2 butylphenylphosphinate aluminum

[0045] The first step: the synthesis of dibutyl phenylphosphonite

[0046] In a four-neck flask equipped with stirring, condensation, and drying devices, add 32.4 g of butanol, 20.2 g of triethylamine, and 110 ml of 1,2-dichloroethane, start stirring, and cool to 3 ° C in an ice-water bath. Slowly add 35.7g of phenylphosphorous dichloride dissolved in 1,2-dichloroethane solution dropwise into the funnel, and the drop is completed in about 2.5 hours; keep at 2-8°C, monitor the reaction by PNMR, and stop the reaction after about 3 hours. After the reaction was completed, the generated solid was filtered off, the solvent and excess butanol were spun off, and the obtained product was purified by distillation under reduced pressure, and the 121-124°C / 12mmHg fraction was intercepted. By weighing, 42.2 g of the product was obtained, and the product yield was 83.0%.

[0047] The second step: the synthesis of phen...

Embodiment 3

[0050] In a flask equipped with a stirring, condensing, and drying device, take 40.1 g of the phenylbutyl phosphonate obtained in step 2, add 130 ml of N, N-dimethylformamide, and 38.9 g of aluminum trichloride, and start stirring device, under the protection of nitrogen, the temperature was raised to 117°C, the chlorobutane generated in the reaction was collected, and the reaction was monitored by PNMR. The reaction was completed after 3 hours of reaction, cooled down, filtered, and the filter cake was washed with acetonitrile and water, dried, and pulverized to obtain butyl 30.6g of aluminum phenyl phosphinate, the total yield of product is 74.0%. The synthesis of embodiment 3 o-tolyl-methyl phosphinate zinc

[0051] The first step: the synthesis of dimethyl o-methylphenylphosphonite

[0052] In a four-necked flask equipped with a stirring, condensing, and drying device, add 19.0 g of methanol, 15.8 g of pyridine, and 110 ml of 1,2-dichloroethane, start stirring, cool to 3°...

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Abstract

The invention discloses a synthesis process of a phosphinate containing alkylaryl in a molecular structure. The phosphinate has the structure as shown in the specification, wherein R1 represents the alkyl of C1-C6, R2 represents hydrogen or the alkyl of C1-C5, and M represents aluminum, zinc, tin (II) or iron; phosphinate is prepared from raw materials aryl phosphorus dichloride and C1-C6 alkanol by virtue of three reactions of esterification, rearrangement and salifying precipitation. Compared with the traditional process in which olefins and phosphinic acid or the metal salts are taken as the raw materials and the synthesis method of free radical addition is adopted, the synthesis process of phosphinate containing alkylaryl in the molecular structure has the advantages that high-pressure reactions are avoided, the operations are simple, the raw materials are richer in source, and the synthesis process is suitable for industrial production.

Description

technical field [0001] The invention relates to the synthesis of an organic phosphinate flame retardant, in particular to a synthesis method of the phosphinate flame retardant containing aryl and alkyl groups in its molecular structure. Background technique [0002] Organic phosphinate flame retardant products are widely used in thermoplastics such as PA, PBT, PET, fibers and textiles, thin-walled electronic components, transparent sheets and films. It has low density and a small amount of flame retardants. It has better mechanical properties, better color, lower smoke density, and higher tracking index value (up to 600V) compared to it. It has a good application prospect in the electrical and electronic industry. [0003] The traditional synthesis process of alkyl phosphinate is generally prepared by reaction of hypophosphorous acid or its alkali metal salt and corresponding olefin in the presence of free radical initiator. For example, in U.S. Patent No. 6,242,642, olefin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 杨锦飞
Owner NANJING JINYUAN FLAME RETARDANT TECH
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