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Method for preparing phosphite ester compounds through reactive rectification coupling

A technology of phosphite and reactive distillation, which is applied in the field of chemical production technology, can solve the problems of increased production cost, sedimentation blockage, viscosity increase, etc., and achieve the effects of increasing production rate, avoiding blockage of equipment, and speeding up the reaction speed

Active Publication Date: 2014-04-16
CHINA TIANCHEN ENG +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For the currently disclosed process of preparing phosphite compounds by adding an acid-binding agent, since the acid-binding agent reacts with the HCl produced in the reaction to generate a large amount of solid ammonia (amine) hydrochloride, the viscosity of the reaction solution system increases , prone to sedimentation and clogging, and in order to obtain liquid products, subsequent liquid-solid separation techniques such as filtration and centrifugation are required, which increases production costs

Method used

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  • Method for preparing phosphite ester compounds through reactive rectification coupling

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 10kg of phenol (reactant 1A) was added to the reactor (2). 4.42 kg of phosphorus trichloride (reactant 2B) was sent to the mixer (5) by metering pump. The temperature of the reaction kettle (2) is 160°C, and the pressure is 1KPag. The feed rate of phosphorus trichloride (reactant 2B) is 1 l / h, and the circulation flow rate of the circulation pump (4) is 12 l / h. The inert gas (C) is high-purity nitrogen with a flow rate of 0.5kg / h, which is fed into the reactor (2) through the sparger (3). The condensing temperature of the heat exchanger 2 (8) is 35° C., and the condensate is refluxed to the top of the tower (1). After reacting for 6 hours, samples were taken for gas chromatography analysis, and the conversion rate of phosphorus trichloride (reactant 2B) was 100%, and the yield of triphenyl phosphite (E) was 94%.

Embodiment 2

[0048] 10kg of phenol (reactant 1A) was added to the reactor (2). 4.42 kg of phosphorus trichloride (reactant 2B) was sent to the mixer (5) by metering pump. The temperature of the reaction kettle (2) is 180°C, and the pressure is 1KPag. The feed rate of phosphorus trichloride (reactant 2B) is 1 l / h, and the circulation flow rate of the circulation pump (4) is 20 l / h. The inert gas (C) is high-purity nitrogen with a flow rate of 1kg / h, which is fed into the reactor (2) through the distributor (3). The condensing temperature of the heat exchanger 2 (8) is 35° C., and the condensate is refluxed to the top of the tower (1). After reacting for 6 hours, samples were taken for gas chromatography analysis, and the conversion rate of phosphorus trichloride (reactant 2B) was 100%, and the yield of triphenyl phosphite (E) was 90%.

Embodiment 3

[0050] 10kg m-cresol (reactant 1A) was added to the reactor (2). 3.84 kg of phosphorus trichloride (reactant 2B) was sent to the mixer (5) by metering pump. The temperature of the reaction kettle (2) is 150°C, and the pressure is 1KPag. The feed rate of phosphorus trichloride (reactant 2B) is 1 l / h, and the circulation flow rate of the circulation pump (4) is 20 l / h. The inert gas (C) is high-purity nitrogen with a flow rate of 0.5kg / h, which is fed into the reactor (2) through the distributor (3). The condensing temperature of the heat exchanger 2 (8) is 35° C., and the condensate is refluxed to the top of the tower (1). After reacting for 10 hours, samples were taken for gas chromatography analysis, the conversion rate of phosphorus trichloride (reactant 2B) was 100%, and the yield of tri-m-cresyl phosphite (E) was 95%.

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Abstract

The invention relates to a method for synthesizing phosphite ester compounds through esterification. Generally, phosphorus halide and alcohol or phenol are adopted for reaction. Taking monohydric alcohol as an example, the reaction equation is as follows: PCl3+3R-OH->P-(O-R)3+3HCl, wherein R is organic group, such as alkane, cycloparaffin, arene and the like. The equipment for the method comprises a reaction kettle, a tower, a circulating pump, a mixer, a heat exchanger and the like. The method has the beneficial effects that HCl generated by reaction is removed timely through the action of reactive rectification coupling, so that the reaction speed is greatly improved, ammonia hydrochloride or amine hydrochloride is prevented from generating due to addition of acid-binding agent, and the production cost of the existing technology is greatly lowered.

Description

technical field [0001] The invention belongs to the technical field of chemical production technology, and in particular relates to a process method for preparing phosphite compounds coupled with reactive distillation. Background technique [0002] Phosphite compounds are important organic chemical intermediates, which can be widely used in the production of brighteners, lubricants, antioxidants, organophosphorus pesticides, and organophosphorus metal complexes in the hydrogen cyanation reaction catalytic system. synthesis. At present, phosphorus trichloride and alcohol are used as raw materials at home and abroad, and inorganic ammonia (commonly used as liquid ammonia) or organic amines (commonly used as dimethylaniline, triethylamine, etc.) are used as acid-binding agents. Solvent for esterification reaction to prepare. [0003] US 3337657 reports the preparation of triethyl phosphite by the reaction of phosphorus trichloride and absolute ethanol in the presence of certa...

Claims

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Application Information

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IPC IPC(8): C07F9/145
CPCY02P20/10Y02P20/582
Inventor 王聪郑仁赵敏伟李荣杨克俭姚立东梁军湘赵斌屈阁许景洋闫伟兰杰刘晶赵丽丽郭萌霍瑜姝
Owner CHINA TIANCHEN ENG
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