CN109516446A - A kind of production method of high-purity yellow phosphorus - Google Patents
A kind of production method of high-purity yellow phosphorus Download PDFInfo
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- CN109516446A CN109516446A CN201811638601.XA CN201811638601A CN109516446A CN 109516446 A CN109516446 A CN 109516446A CN 201811638601 A CN201811638601 A CN 201811638601A CN 109516446 A CN109516446 A CN 109516446A
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- Prior art keywords
- yellow phosphorus
- purity
- filler
- production method
- sulfur
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/04—Purification of phosphorus
- C01B25/047—Purification of phosphorus of yellow phosphorus
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of production methods of high-purity yellow phosphorus, include the following steps: to distill the yellow phosphorus of sulfur-containing impurities in the high purity quartz distillation column equipped with filler, yellow phosphorus and filler weight ratio are at (2-5): 1, distillation column bottom is passed through inert gas, and 240-320 DEG C of vapo(u)rizing temperature；220-280 DEG C of fraction, which is collected, in quartz distillation top end obtains the yellow phosphorus of high-purity low-sulfur through circulating water to 20-25 DEG C.Wherein: filler as described in step (1) is that chromium, cobalt, manganese, iron, copper, one or more metal fillers of nickel and high purity quartz θ ring are mixed, metal filler and high purity quartz θ ring weight ratio are at (5-7): 1, the purity > 99.999% of metal filler.Present invention purity is high, low-sulfur, process flow are short, highly-safe.
Description
Technical field
The present invention relates to chemical technology field, in particular to a kind of production method of high-purity yellow phosphorus.
Background technique
High-purity yellow phosphorus is widely used in the fields such as compound semiconductor, light emitting diode, solar battery.In synthesis phosphatization
In indium (InP), gallium phosphide (GaP) compound semiconductor, 99.9999% need to be greater than for the purity of phosphorus source, especially for impurity
Sulfur content need to be less than 0.1ppm or less.
It is influenced by factors such as raw material and manufacturing conditions, normal sulfur-bearing, organic impurities, silicon and gold in industrial yellow phosphorus product
Belong to impurity etc..Existing purification process mainly has chemical method and absorption method, and chemical method mainly uses oxidant to carry out oxygen to yellow phosphorus
Change, deviate from impurity therein from yellow phosphorus, absorption method mainly using there is stronger adsorption capacity such as active carbon as adsorbent,
Partial impurities are made to separate, remove from yellow phosphorus.
China Patent Publication No. CN103588185A discloses a kind of yellow phosphorus purification process, using certain density water solubility
Organic amine aqueous solution comes into full contact with as desulfurizing agent in 50-85 DEG C of temperature, under agitation with liquid-state industrial yellow phosphorus, and industry is yellow
Sulfur impurity in phosphorus enters aqueous solution, to realize the separation removal with yellow phosphorus.The yellow phosphorus product sulfur content that this method obtains is most
Low is 35ppm, is not able to satisfy semicon industry demand.
German patent DE 76482 discloses that a kind of to use weight be the concentrated sulfuric acid of yellow phosphorus weight 15-18% and yellow phosphorus in spy
In the reactor of matter after hybrid reaction the yellow phosphorus of isolated low sulfur concentration method, this method is during using the concentrated sulfuric acid
Fierceness dilution heat release is easy to happen explosion danger, increases operational danger, the yellow phosphorus product sulfur content that this method obtains is still big
In 100ppm, sulphur removal effect is limited.
Summary of the invention
A kind of purity is high for there is provided it is an object of the invention to overcome disadvantages mentioned above, low-sulfur, process flow be short, safety
The production method of high high-purity yellow phosphorus.
A kind of production method of high-purity yellow phosphorus of the invention, includes the following steps:
(1) yellow phosphorus of sulfur-containing impurities is distilled in the high purity quartz distillation column equipped with filler, yellow phosphorus and filler weight
Ratio is measured at (2-5): 1, it distills column bottom and is passed through inert gas, 240-320 DEG C of vapo(u)rizing temperature；
(2) 220-280 DEG C of fraction is collected in quartz distillation top end obtain high-purity through circulating water to 20-25 DEG C
The yellow phosphorus of low-sulfur.
A kind of production method of above-mentioned high-purity yellow phosphorus, in which: filler described in step (1) be chromium, cobalt, manganese, iron,
Copper, one or more metal fillers of nickel and high purity quartz θ ring are mixed, metal filler and high purity quartz θ ring weight
Than at (5-7): 1, the purity > 99.999% of metal filler.
A kind of production method of above-mentioned high-purity yellow phosphorus, in which: preferred 270-310 DEG C of the vapo(u)rizing temperature.
The production method of above-mentioned a kind of high-purity yellow phosphorus, in which: the yellow phosphorus and filler weight are than preferred (3-4): 1.
The production method of above-mentioned a kind of high-purity yellow phosphorus, in which: the inert gas is argon gas or nitrogen.
A kind of production method of above-mentioned high-purity yellow phosphorus, in which: preferred 260-275 DEG C of fraction in step (2).
Compared with prior art, the present invention having apparent beneficial effect, as can be known from the above technical solutions: the present invention is utilized
Under an inert gas, when yellow phosphorus steam is by distillation filler, in metal filler mixed fillers layer surface chemistry occurs for sulphur impurity
Absorption, effectively removes the sulphur impurity in yellow phosphorus；Additionally by distillation, the temperature of fraction is collected in control, organic impurities in yellow phosphorus,
Metal impurities are removed.Yellow phosphorus especially sulphur impurity removal effect through the present invention after purification is good, obtained yellow phosphorus sulfur content
99.9999% can be greater than down to 100ppb, product purity.Product quality is able to satisfy compound semiconductor and wants to the quality of phosphorus source
It asks.And present invention process is simple, highly-safe.
Specific embodiment
Embodiment 1-6
A kind of production method of high-purity yellow phosphorus, includes the following steps:
(1) yellow phosphorus of sulfur-containing impurities is distilled in the high purity quartz distillation column equipped with filler, yellow phosphorus and filler weight
Ratio is measured at (2-5): 1, it distills column bottom and is passed through inert gas, 240-320 DEG C of vapo(u)rizing temperature；
(2) 220-280 DEG C of fraction is collected in quartz distillation top end obtain high-purity through circulating water to 20-25 DEG C
The yellow phosphorus of low-sulfur.
According to the above method, specific process parameter is shown in Table 1 to embodiment 1-6.
The analysis of sulfur content is detected by ICP-MS in the yellow phosphorus that embodiment 1-6 is obtained, and testing result is shown in Table 2
The process conditions of 1 embodiment 1-6 of table
The testing result of 2 embodiment 1-6 of table
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form, appoint
What is to the above embodiments according to the technical essence of the invention any simply to repair without departing from technical solution of the present invention content
Change, equivalent variations and modification, all of which are still within the scope of the technical scheme of the invention.
Claims (6)
1. a kind of production method of high-purity yellow phosphorus, includes the following steps:
(1) yellow phosphorus of sulfur-containing impurities is distilled in the high purity quartz distillation column equipped with filler, yellow phosphorus and filler weight ratio
At (2-5): 1, distillation column bottom is passed through inert gas, and 240-320 DEG C of vapo(u)rizing temperature；
(2) 220-280 DEG C of fraction is collected in quartz distillation top end obtain high-purity low-sulfur through circulating water to 20-25 DEG C
Yellow phosphorus.
2. a kind of production method of high-purity yellow phosphorus as described in claim 1, in which: filler as described in step (1) be chromium,
Cobalt, manganese, iron, copper, one or more metal fillers of nickel and high purity quartz θ ring are mixed, metal filler and high-purity stone
English θ ring weight ratio is at (5-7): 1, the purity > 99.999% of metal filler.
3. a kind of production method of high-purity yellow phosphorus as described in claim 1, in which: preferred 270-310 DEG C of the vapo(u)rizing temperature.
4. a kind of production method of high-purity yellow phosphorus as described in claim 1, in which: the yellow phosphorus and filler weight are than preferred
(3-4): 1.
5. a kind of production method of high-purity yellow phosphorus as described in claim 1, in which: the inert gas is argon gas or nitrogen.
6. a kind of production method of high-purity yellow phosphorus as described in claim 1, in which: the preferred 260-275 of fraction in step (2)
℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811638601.XA CN109516446A (en) | 2018-12-29 | 2018-12-29 | A kind of production method of high-purity yellow phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811638601.XA CN109516446A (en) | 2018-12-29 | 2018-12-29 | A kind of production method of high-purity yellow phosphorus |
Publications (1)
| Publication Number | Publication Date |
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| CN109516446A true CN109516446A (en) | 2019-03-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201811638601.XA Pending CN109516446A (en) | 2018-12-29 | 2018-12-29 | A kind of production method of high-purity yellow phosphorus |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5173173A (en) * | 1990-09-28 | 1992-12-22 | Union Oil Company Of California | Trace contaminant removal in distillation units |
| CN109052352A (en) * | 2018-10-10 | 2018-12-21 | 湖北兴福电子材料有限公司 | A kind of method of industrial yellow phosphorus production electron-level phosphoric acid |
-
2018
- 2018-12-29 CN CN201811638601.XA patent/CN109516446A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5173173A (en) * | 1990-09-28 | 1992-12-22 | Union Oil Company Of California | Trace contaminant removal in distillation units |
| CN109052352A (en) * | 2018-10-10 | 2018-12-21 | 湖北兴福电子材料有限公司 | A kind of method of industrial yellow phosphorus production electron-level phosphoric acid |
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Application publication date: 20190326 |