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A high-pressure oxidation synthesis process and equipment for trihydroxymethylphosphine oxide

A technology of hydroxymethylphosphine oxide and synthesis process, which is applied in the field of chemical production, can solve problems such as lack of production equipment and process routes, restrict the development of industrial scale, and serious environmental pollution, and achieve great social benefits, economic value, and operational strength The effect of small size and simple process route

Active Publication Date: 2016-06-22
湖北省兴发磷化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the lack of reasonable and efficient production equipment and process routes, the PH 3 The energy consumption of synthesizing THPO as a raw material is high, the production cost is high, and the environmental pollution is serious, which restricts its industrial-scale development

Method used

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  • A high-pressure oxidation synthesis process and equipment for trihydroxymethylphosphine oxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 500L methanol and 400kg paraformaldehyde into a 1000L pressure cooker, pass in nitrogen protection, stir to raise the temperature to 85°C, and pass in 160kgPH 3 Gas, pressurized to 3.5~4.0MPa, reacted for 1.5h, lowered to normal temperature and pressure; transferred the material to a 1000L oxidation kettle, 3 The throughput of / min is 28m 3 The air, heating and stirring, raised the temperature to 95 ° C, and after 5 hours of reaction, it was cooled to room temperature; the material was filtered through a filter, and the filtrate was transferred to a precipitation kettle, and the desolvation temperature was 65 ~ 70 ° C, and the solvent was dehydrated ( The solvent is rectified and recycled by the rectification tower), and when the water content of the material reaches 1.0~1.2%, the precipitation is stopped, and the material is transferred to the finished product tank. Gained THPO580Kg, the product purity is more than 99%, and the yield is more than 95%.

Embodiment 2

[0020] Add 645L ethylene glycol monoethyl ether and 322kg paraformaldehyde into a 1000L pressure cooker, pass in nitrogen protection, stir to raise the temperature to 68°C, and pass in 252kgPH 3 Gas, pressurize to 4.0MPa, react for 3h, drop to normal temperature and pressure; transfer the material to a 1000L oxidation kettle, add 32.5L peroxydicarbonate with a concentration of 80%, heat and stir, raise the temperature to 55°C, and react for 3.8 After h, it is lowered to room temperature; the material is filtered through a filter, and the filtrate is transferred to a desolventization kettle, and the desolventization temperature is 68°C, and the solvent is de-dried (the solvent is rectified and recycled by a rectification tower), and the material water When the content reaches 1.0~1.2%, stop the precipitation and transfer the material to the finished product tank. Gained THPO740Kg, product purity more than 99%, yield more than 95%.

Embodiment 3

[0022] Add 400L of methanol, 120L of dichloromethane and 400kg of paraformaldehyde into a 1000L pressure cooker, pass in nitrogen protection, stir to raise the temperature to 85°C, and pass in 160kgPH 3 Gas, pressurized to 3.5~4.0MPa, reacted for 1.5h, lowered to normal temperature and pressure; transferred the material to a 1000L oxidation kettle, 3 Influx of / min into 20m 3 Oxygen, heat and stir, heat up to 55°C, and after 5 hours of reaction, it will be cooled to room temperature; the material is filtered through a filter, the filtrate is transferred to a precipitation kettle, and vacuum distillation is carried out. The precipitation temperature is 65~70°C, and the solvent is dehydrated ( The solvent is rectified and recycled by the rectification tower), and when the water content of the material reaches 1.0~1.2%, the precipitation is stopped, and the material is transferred to the finished product tank. Gained THPO590Kg, product purity more than 98%, yield more than 95%. ...

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Abstract

The invention relates to a high-pressure oxidation synthesis process and equipment for trishydroxymethylphosphine oxide (THPO). The production process includes the following steps: adding organic solvent and paraformaldehyde into the high-pressure reaction kettle, feeding nitrogen protection, stirring to raise the temperature to 60~100°C, feeding PH3 gas to pressurize, and maintaining the pressure inside the kettle at 3.0~5.0MPa, After reacting for 1~3h, lower to normal pressure and normal temperature; transfer all the materials to an oxidation kettle, add an oxidant, heat up to 30~120°C, stir and react for 3~6h, then drop to room temperature; filter the materials through a filter, and transfer the filtrate to Desolventizing kettle, vacuum distillation, the desolventizing temperature is 55~85℃, when the moisture content of the material is less than 2%, the material is transferred to the finished product tank. The invention has the advantages of simple process route, few procedures and low operation intensity; no catalyst and low production cost; comprehensively utilizes the by-product PH3 in the production of sodium hypophosphite; has no pollution to the environment and is environmentally friendly.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a production process and production equipment for synthesizing trihydroxymethylphosphine oxide by high-pressure oxidation using phosphine gas as a raw material. Background technique [0002] With the growing demand for flame retardant and disaster prevention around the world, the improvement of flame retardant regulations, the increasingly stringent safety and environmental protection standards and the increase in the application of plastic products, the demand for the entire flame retardant market will reach 2.2 million tons by 2014. The global market capacity of flame retardants is expected to reach 680,000 tons. At present, many flame retardants produced and used in China are inorganic and halogen-containing flame retardants. However, due to the presence of halogen-containing flame retardants, smoke, corrosive gases and toxic gases are emitted during combustion....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53
Inventor 李永刚王明峰宋宏图马会娟田路
Owner 湖北省兴发磷化工研究院有限公司
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