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Preparation method of pentaerythritol diphosphate

A pentaerythritol and bisphosphonate technology is applied in the field of preparation of pentaerythritol-type bisphosphonates, and can solve the problems of easy decomposition of products, high reaction temperature, difficulty in industrialized large-scale production, etc., and achieves short reaction time, reduced reaction temperature, The effect of shortened time

Pending Publication Date: 2020-09-01
ZHEJIANG WANSHENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The yield of this method is between 55% and 65%, and the reaction temperature of this route is too high, and the product is easy to decompose under high temperature for a long time, resulting in low yield and a gel-like substance, which is difficult to carry out large-scale industrial production

Method used

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  • Preparation method of pentaerythritol diphosphate

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preparation example Construction

[0025] The invention provides a kind of preparation method of pentaerythritol type diphosphate, comprises the following steps:

[0026] (1) under the action of a catalyst, phosphorus oxychloride and phenolic compounds are subjected to the first esterification reaction to obtain phosphoryl dichloride compounds;

[0027] (2) Under vacuum and decompression conditions, sequentially add phosphoryl dichloride compound and acid-binding agent to the pentaerythritol solution to carry out the second esterification reaction to obtain pentaerythritol-type bisphosphate.

[0028] In the present invention, under the action of a catalyst, phosphorus oxychloride and phenolic compounds are subjected to a first esterification reaction to obtain phosphorus oxydichloride compounds. In the present invention, the catalyst is preferably a Lewis acid; the Lewis acid is preferably one or more of titanium tetrachloride, magnesium chloride and aluminum chloride; the amount of the catalyst is preferably t...

Embodiment 1

[0045] Add 460kg (3.0kmol) of phosphorus oxychloride and 2kg of magnesium chloride into the reaction kettle and slowly raise the temperature to 80-85°C, start to add 94kg (1kmol) of phenol dropwise, and finish the dropwise addition in about 1 hour. Insulate for 2 hours, after the reaction is complete, lower the temperature to room temperature and slowly distill phosphorus oxychloride under reduced pressure. Collect the 110-120°C fraction under the condition of a temperature of 5-10kPa to obtain 190kg of phenoxyphosphoryl dichloride intermediate, yield: 90%, content: 98% (gas chromatography);

[0046] Add 61.3kg (0.45kmol) of pentaerythritol and 100kg of xylene into the reaction kettle, open the reflux condenser, the cooling temperature of the condenser is -5~0℃, in order to prevent the toluene from being taken away, add phosphoryl dichloride dropwise under reduced pressure Compound 190kg (0.9kmol), vacuum degree 70 ~ 75kPa, exothermic heat is obvious during the dropping proces...

Embodiment 2

[0048] Add 950kg (6.20kmol) of phosphorus oxychloride and 4kg of magnesium chloride into the reaction kettle and slowly raise the temperature to 80-85°C, start to add 190kg (2kmol) of phenol dropwise, and finish the dropwise addition in about 2 hours. Keep warm for 3 hours. After the reaction is complete, lower the temperature to room temperature and slowly distill phosphorus oxychloride under reduced pressure. The vacuum degree is 30-40kPa. Distill to 90-95°C to stop the distillation. The recovered phosphorus oxychloride is reused, and then the The 110-120°C fraction was collected under the condition of ~10kPa to obtain 386kg of phenoxyphosphoryl dichloride intermediate, yield: 91.5%, content: 98.2% (gas chromatography).

[0049] Add 130kg (0.95kmol) of pentaerythritol and 200kg of xylene into the reaction kettle, open the reflux condenser, the cooling temperature of the condenser is -5~0°C, to prevent the xylene from being taken away, add phosphoryl dichloride dropwise under ...

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Abstract

The invention relates to the technical field of organic synthesis, and provides a preparation method of pentaerythritol diphosphate. The phosphoryl dichloride compound is prepared from a phenolic compound and phosphorus oxychloride under the condition of a catalyst, the yield of the phosphoryl dichloride compound is high, the activity of the phosphoryl dichloride compound is high, and the next step of reaction can be directly carried out without drying; then the phosphoryl dichloride compound is reactd with pentaerythritol under the vacuum pressure reduction condition, acid generated in the reaction can be rapidly removed under the vacuum pressure reduction condition, and the reaction can be carried out in the forward direction; furthermore, a phosphoryl dichloride compound is dropwise added, after dropwise adding is completed, esterification can be completed basically by one acyl chloride, and at the moment, an acid-binding agent is added, so that esterification of a second acyl chloride is facilitated, and the reaction time is greatly shortened; and the reaction temperature can be reduced under the vacuum decompression condition, the problems of acidolysis of pentaerythritol diphosphate and reaction with hydrogen chloride are avoided, the reaction safety and operability are improved, and the reaction efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of pentaerythritol type bisphosphate. Background technique [0002] Pentaerythritol bisphosphate is widely used as an additive flame retardant due to its high flame retardancy, low volatility, and good compatibility with epoxy resins. Adding a certain amount of pentaerythritol-type bisphosphate flame retardants to polyurethane and polyamide engineering plastics can greatly improve the flame retardant properties of the products. Many manufacturers of flame retardants are producing them, and their application prospects are very good. [0003] The commonly used synthetic method of pentaerythritol-type bisphosphate is as follows: in the patent CN201310255001.6, pentaerythritol and phosphorus oxychloride are used to react for a long time to produce pentaerythritol diphosphoryl chloride. Carry out esterification reaction, make the compound of spiro ring ...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65744
Inventor 吕云兴李东亮方剑王秋伟
Owner ZHEJIANG WANSHENG
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