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Phosphate-phosphonate preparation method

A technology of phosphoric acid ester phosphonate and alcohol phosphonate, applied in the high-purity field, can solve the problems of reduced yield of target compounds, troublesome hydrogen peroxide treatment, low generation efficiency, etc., shortening temperature and time, avoiding explosion danger, The effect of shortening the reaction time

Inactive Publication Date: 2018-12-21
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem that this method exists is that the kind of the phosphonate ester of raw material is received restriction, when the phosphonate ester with primary hydroxyl is used as raw material, there is no problem in the reaction process, but when the phosphonate ester with secondary hydroxyl or tertiary hydroxyl is used as As a raw material, its reactivity with compounds having a pentavalent P(=O)-Cl bond is very low, resulting in a reduced yield of the target compound
In addition, the treatment of excess hydrogen peroxide after hydrogen peroxide oxidation is very troublesome. Improper handling is likely to cause explosion safety hazards. The time for hydrogen peroxide oxidation is more than 4 hours, and the reaction temperature is required to be above 40°C. It is not easy to oxidize at low temperature, and the oxidation time is too long , the generation efficiency is not high

Method used

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Effect test

Embodiment 1

[0086] Embodiment 1: the preparation of neopentylphosphorous chloride

[0087] Neopentyl glycol (50g, 0.48mol) and toluene (100g) were added into a four-necked flask and stirred, protected by nitrogen, cooled to 15-20°C, and phosphorus trichloride (75g, 0.55mol, neopentyl glycol The molar ratio to phosphorus trichloride is 1:1.15) and added dropwise for 1 hour, and kept warm (15-20°C) for 15 minutes after the drop, the solution gradually became clear, and the vacuum was slowly turned on, and the acid was pumped under reduced pressure to obtain neopentyl Phosphorus chloride 78g, yield 95%;

Embodiment 2

[0088] Embodiment 2: the preparation of neopentylphosphorous chloride

[0089] Neopentyl glycol (150g, 1.44mol), toluene (300g), add to a four-necked flask and stir, protect with nitrogen, cool down to 15-20°C, add phosphorus trichloride (225g, 1.64mol, neopentyl glycol) dropwise The molar ratio to phosphorus trichloride is 1:1.14) and added dropwise for 1 hour, and kept warm (15-20°C) for 15 minutes after the drop, the solution gradually became clear, and the vacuum was slowly turned on, and acid was pumped under reduced pressure to obtain neopentyl Phosphorus chloride 240g, yield: 97%.

Embodiment 3

[0090] Embodiment 3: the preparation of neopentylphosphorous chloride

[0091] Neopentyl glycol (200g, 1.91mol), toluene (400g), add to a four-necked flask and stir, protect with nitrogen, cool to 15-20°C, add phosphorus trichloride (300g, 2.19mol, neopentyl glycol) dropwise The molar ratio to phosphorus trichloride is 1:1.15) and added dropwise for 2 hours, and kept warm (15-20°C) for 60 minutes after dropping, the solution gradually became clear, and the vacuum was slowly turned on, and the acid was pumped under reduced pressure to obtain neopentyl Phosphorus chloride 320g, yield: 96%.

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Abstract

The invention relates to a phosphate-phosphonate preparation method, which comprises the following steps: performing condensation and dehydration reaction on neopentyl phosphite and alcohol phosphonate in the presence of an esterification catalyst, then adding ozone for oxidation, and distilling a solvent under reduced pressure to obtain the phosphate-phosphonate, the neopentyl phosphite being generated by hydrolyzing neopentyl phosphorochloridite. According to the method, use of a triethylamine acid binding agent is avoided, so that problems about recovery and pollution of a large amount of triethylamine hydrochloride are reduced; the mild ozone is adopted as an oxidizer, so that simplicity and convenience are ensured, explosion dangers of hydrogen peroxide are avoided, the reaction condition is mild and easy to control, and the ozone subjected to aftertreatment can be conveniently and rapidly treated directly by illumination; time for oxidation reaction is greatly shortened, the reaction temperature is low, and the purity and the yield of an obtained product are high, and are greatly improved compared with those achieved by a conventional process.

Description

technical field [0001] The invention relates to the technical field of fine chemical production, and specifically designs a high-purity, high-yield phosphate-phosphonate preparation method. Background technique [0002] Phosphate-phosphonate has multi-functionality such as plasticizing and flame retardant. It is widely used, has good development potential and good market space. Accelerating the development of phosphonate series agent technology is to further promote plasticizing in my country. An important way for the rapid development of flame retardants. [0003] There are many inventions related to the preparation or synthesis of phosphate-phosphonate, for example (see CN101048420A (application number 200580037224.9) for the first three parts): [0004] US4697030 discloses a kind of synthetic method of phosphoric acid ester-phosphonic acid ester, under the condition that Lewis acid catalyst such as magnesium chloride and triethylamine as hydrogen chloride remover coexist,...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65746
Inventor 王秋伟牛丽丹金译平王咪咪
Owner ZHEJIANG WANSHENG