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Production of electronic grade yellow phosphorus

A production method and electronic-grade technology, applied in the field of elemental phosphorus, can solve problems such as harsh conditions, poor separation effect, and long reaction time, and achieve the effects of easy industrialization, convenient filtration, and short reaction time

Inactive Publication Date: 2007-10-03
JINGYI SCI & TECH GUIYANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Physical methods include distillation, adsorption, ion exchange, extraction, etc. Distillation and extraction are commonly used, but because phosphorus and arsenic are elements of the same main group, their physical and chemical properties are relatively similar, and it is difficult to achieve a high removal rate; yellow phosphorus also contains Contains a variety of inorganic impurities, and the separation effect of adsorption method is poor
In recent years, many patents have been applied for the production method of electronic-grade yellow phosphorus at home and abroad. Among these applications, the more important one is No. 03117527.9 "Production method of high-purity yellow phosphorus". This patent technology belongs to the distillation oxidation method. The disadvantages are: the operation process needs to be distilled under reduced pressure and isolated from the air, and the conditions are harsh; sulfuric acid is used in the production process, which greatly reduces the safety of the operation; there is also No. 03135191.3 "Production Process of Electronic Grade Red Phosphorus" The oxidation method that adopts in the method, its shortcoming is: its oxidizing agent is strong oxidizing strong acid, and strong oxidizing strong acid also will oxidize yellow phosphorus when oxidizing other impurity, and its product yield is low; Inability to achieve sufficient contact resulting in longer reaction times

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 4kg of industrial yellow phosphorus into a mixed liquid containing 3.74kg of pure water and 0.98kg of analytically pure nitric acid, heat and stir, control the stirring speed at 45-75r / min, add surfactant oπ-10, add oπ The amount of -10 is 0.5% of the mass of yellow phosphorus. When the temperature rises to 75-85°C, add 300ml of 10% reducing agent iodine salt and molybdate, and 40ml of 5% oxidation enhancer potassium permanganate and dichromate Potassium acid, stirring; if a small amount of foam is generated during the reaction, a small amount of antifoaming agent water-soluble silicone oil can be added. After reacting for about 1.5h, the upper liquid was removed. Respond like this 3 times. After the reaction, add 3.74kg of pure water to heat and stir. When the temperature rises to 75-85°C, add 0.98kg of hydrochloric acid and 50ml of 15% sodium silicate solution, and stir for about 1.5h; Wash with water, heat and stir until the upper liquid wash is neutral, and me...

Embodiment 2

[0018] Put 8kg of industrial yellow phosphorus into a mixed liquid containing 7.48kg of pure water and 1.96kg of analytically pure nitric acid, heat and stir, control the stirring speed at 55-85r / min, add surfactant lignosulfonate, add The amount of lignosulfonate is 1% of the mass of yellow phosphorus. When the temperature rises to 75-85°C, add 700ml of 10% reducing agent iodine salt and molybdate, and 80ml of 5% oxidation enhancer potassium permanganate Stir with sodium dichromate; if there is a small amount of foam during the reaction, add a small amount of defoamer foam enemy MPE; react for about 1.5 hours, remove the upper liquid, and repeat this 4 times; add 7.48kg of pure water after the reaction Heat and stir, when the temperature rises to 75-85°C, add 1.96kg of phosphoric acid and 100ml of 15% sodium silicate solution, and stir for about 1.5h; remove the upper liquid, wash with 85°C hot pure water, heat and stir, Wash until the upper liquid is neutral, and measure it ...

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Abstract

A process for preparing electronic-class yellow phosphorus includes such steps as adding industrial yellow phosphorus to the mixture of oxidizing strong acid and purified water, heating while stirring, adding oxidizing strong acid, reducer, oxidizing enhancer and surfactant, heating while stirring, removing upper liquid layer, repeating the steps 2-4 times, adding non-oxidizing acid, sodium silicate and purified water, heating while stirring, removing upper liquid layer, washing with hot purified water, heating while stirring, adding purified activated carbon, heating while stirring, and filtering.

Description

technical field [0001] The present invention relates to elemental phosphorus, in particular to yellow phosphorus, especially electronic grade yellow phosphorus. Background technique [0002] At present, there are about 25 technical routes for the production of electronic-grade yellow phosphorus at home and abroad, which can be summarized into physical methods, chemical methods and other methods. Physical methods include distillation, adsorption, ion exchange, extraction, etc. Distillation and extraction are commonly used, but because phosphorus and arsenic are elements of the same main group, their physical and chemical properties are relatively similar, and it is difficult to achieve a high removal rate; yellow phosphorus also contains Contains a variety of inorganic impurities, and the separation effect of adsorption method is poor. In recent years, many patents have been applied for the production method of electronic-grade yellow phosphorus at home and abroad. Among the...

Claims

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Application Information

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IPC IPC(8): C01B25/047
Inventor 姜国强
Owner JINGYI SCI & TECH GUIYANG