CN109850860A - The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus - Google Patents
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus Download PDFInfo
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Abstract
The invention discloses the production technologies that electronic grade red phosphorus is converted by depth pickling yellow phosphorus, and industrial yellow phosphorus successively being included the steps that, depth pickling, chlorination, rectifying, hydrogen reducing and constant-pressure and high-temperature convert, obtains the electronic grade red phosphorus that purity is 99.9999%.Above-mentioned technique is by improving traditional industry yellow phosphorus acid cleaning process, on the one hand the relatively mild air agitation of replacement tradition is stirred with mechanical deep, and kettle outside sandwich recycles logical hot water thermal insulating, yellow phosphorus and nitric acid is set to come into full contact with reaction, remove the impurity that the subsequent techniques such as S, C and As not can be removed, and reaction process is not necessarily to additive, improve product purity, the yellow phosphorus rate of recovery greatly improves, increase electronic grade red phosphorus yield, on the other hand replace conventional quartz reaction kettle with the interior enamel cast iron kettle with outside sandwich, reduce production safety hidden danger.
Description
Technical field
The present invention relates to the preparations of element phosphor, and in particular to the preparation of electronic grade red phosphorus (6N), further to by depth
Pickling yellow phosphorus is converted into the production technology of electronic grade red phosphorus.
Background technique
Red phosphorus, molecular formula P4, molecular weight 123.8, the allotrope of white phosphorus, bronzing amorphous powder or blocky solid
Body.Relative density 2.34g/cm3, 590 DEG C of fusing point, 200 DEG C of ignition point or more, not soluble in water, carbon disulfide and organic solvent are micro-
It is dissolved in dehydrated alcohol.Electronic grade red phosphorus is one of the main material for synthesizing phosphorus compound semiconductor, can be used for synthesizing indium phosphide
(LnP), the compound semiconductors such as gallium phosphide (GaP), it is also possible to which the solid-state phosphorus source for making IC doping is widely used in integrated circuit, too
The fields such as positive energy cell piece, crystalline silicon, compound semiconductor, TFT-LCD, preform and optical crystal.
Currently, the method for producing high-purity red phosphorus at present, which is substantially, is converted into red phosphorus using yellow phosphorus (white phosphorus), conversion
Form is roughly divided into two kinds:
(1) normal pressure converts: being usually by carrying out the cooling steam for reducing converter (converter) to phosphorus steam and tail gas
Pressure realizes that high-temperature pressure yellow phosphorus is converted into red phosphorus, as patent CN102556988B discloses " ultra-pure white phosphorus ordinary-pressure conversion side
Method " gradually heats up 6N grades of ultrapure white phosphorus according to gradient, and 14 gradients DEG C are divided into from 170 DEG C to 355 and carry out constant temperature, gradually real
Existing white phosphorus conversion, but the normal pressure method for transformation time is longer, and primary conversion at least needs 137h successively to produce, production operation
More complicated, technological operation difficulty is big.
(2) high pressure converted: it is 300 DEG C or so that high pressure converted, which is in temperature, is carried out under certain pressure, entire heating and pressurization
Process gradually carries out, and 325 DEG C of maximum temperature, being finally filled with inert gas pressure total in container can reach 10 atmospheric pressure
Under gradually convert red phosphorus for yellow phosphorus, will be high-purity if patent CN101214935B discloses " production technology of electronic grade red phosphorus "
Yellow phosphorus is transferred to conversion pot, at 20 DEG C~80 DEG C 1~2kg of filling with inert gas, at 80 DEG C~200 DEG C filling with inert gas 2~
4kg, the not filling with inert gas at 200 DEG C~250 DEG C, 1~2kg of filling with inert gas at 250 DEG C~280 DEG C, 280 DEG C~
1~2kg of filling with inert gas, naturally cools to room temperature at 300 DEG C, obtains 99.9999% high-purity red phosphorus product, but this method is to setting
Relatively high for requiring, there is also security risks for condition of high voltage.
In addition, the production technology of above-mentioned 99.9999% high-purity red phosphorus: yellow phosphorus (white phosphorus) after pickling successively through chlorination,
Rectifying, reduction and conversion and obtain；Wherein, pickling is the pass that electronic grade yellow phosphorus (white phosphorus) is converted into after industrial yellow phosphorus (white phosphorus) cleans
Key process is most important to 99.9999% high-purity red phosphorus of subsequent acquisition.In the prior art, it generallys use toward splendid attire yellow phosphorus and nitre
Argon gas is passed through in the quartzy kettle of acid solution and inert gas is stirred, part acid cleaning process also adds NaI enhancing pickling effect,
But there are still following problems:
1) stirring is insufficient, except the elements effects such as impurity especially As, S and C are undesirable；
2) additive such as NaI etc. is added and brings new impurity；
3) quartz material is easily broken, and there are serious security risks；
4) industrial yellow phosphorus (white phosphorus) be converted into electronic grade yellow phosphorus (white phosphorus) the rate of recovery it is low.
Summary of the invention
The purpose of the present invention is to provide a kind of production technologies that electronic grade red phosphorus is converted by depth pickling yellow phosphorus, solve
Industrial grade yellow phosphorus acid cleaning process is except impurity (especially As, S and C) effect is poor, the yellow phosphorus rate of recovery is low, stirring is not filled in the prior art
Divide and there are problems that security risk.
The technical solution adopted by the present invention to solve the technical problems is:
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, by industrial yellow phosphorus successively through including
(I) depth pickling, and
(II) chlorination, and
(III) rectifying, and
(IV) hydrogen reducing, and
The step of (V) constant-pressure and high-temperature converts obtains the electronic grade red phosphorus that purity is 99.9999%；Wherein:
In step (I), the depth pickling process includes: that will be diluted to the nitric acid that mass fraction is 20% to be added to and install
Continued mechanical stirring is carried out in the enamel cast iron kettle of industrial yellow phosphorus, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and institute
It states impurity in industrial yellow phosphorus sufficiently to react, then reaction product is cleaned with pure water；Wherein, the impurity includes As, S and C, described
The mass ratio of nitric acid and industrial yellow phosphorus is 1:3.
Further, in step (II), the chloride process are as follows: the yellow phosphorus after depth pickling in step (I) is transferred to chlorine
Change in kettle, is passed through chlorine and reacts generation phosphorus trichloride with yellow phosphorus；The phosphorus trichloride volatilization generated under the action of reaction heat, through cold
Liquid phosphorus trichloride is collected after solidifying section；Wherein, the mass ratio of the chlorine and yellow phosphorus is 1:0.29.
Further, in step (III), the rectification working process are as follows: control rectifying column in temperature phosphorus trichloride boiling point with
On, while separating impurity by not having to component volatilization degree difference, the steam of phosphorus trichloride becomes after rising to rectifying column condensation segment
At liquids recovery；It repeats above-mentioned distillation process 3~5 times.
Further, in step (III), temperature is controlled 20~30 DEG C more than phosphorus trichloride boiling point in the rectifying column,
Steam becomes liquids recovery after rising to the condensation segment of rectifying column, repeats above-mentioned distillation process 3~4 times.
Further, in step (III), temperature is controlled 20~25 DEG C more than phosphorus trichloride boiling point in the rectifying column,
Steam becomes liquids recovery after rising to the condensation segment of rectifying column, repeats above-mentioned distillation process 4 times.
Further, in step (IV), the hydrogen reducing process are as follows: be passed through with 5N hydrogen and obtained equipped with step (III) rectifying
Phosphorus trichloride reaction tube in reacted, obtain 6N yellow phosphorus.
Further, in step (V), the constant-pressure and high-temperature conversion procedure are as follows: by the 6N yellow phosphorus that reduction obtains in step (IV)
It is packed into conversion tube, for ladder-elevating temperature to 400 DEG C, conversion obtains 6N red phosphorus；Wherein: the ladder-elevating temperature process are as follows:
180~200 DEG C of constant temperature convert 3~6h, and 200~220 DEG C of constant temperature convert 3~6h, and 220~240 DEG C of constant temperature conversions 3~
6h, 240~260 DEG C of constant temperature convert 3~6h, and 260~300 DEG C of constant temperature convert 3~6h, and 300~350 DEG C of constant temperature convert 3~6h,
350~380 DEG C of 6~12h of constant temperature conversion, 380~400 DEG C of constant temperature conversions 12~for 24 hours.
Further, in step (V), the ladder-elevating temperature conversion process are as follows: 185~195 DEG C of constant temperature convert 3~5h,
205~215 DEG C of constant temperature convert 3~5h, and 225~235 DEG C of constant temperature convert 3~5h, and 245~255 DEG C of constant temperature convert 3~5h, 275~
285 DEG C of constant temperature convert 3~5h, and 315~335 DEG C of constant temperature convert 3~5h, and 365~375 DEG C of constant temperature convert 8~12h, and 385~395
DEG C constant temperature conversion 16~for 24 hours.
Further, in step (V), the ladder-elevating temperature conversion process are as follows: 190 DEG C of constant temperature convert 4h, 210 DEG C of constant temperature
Converting 4h, 230 DEG C of constant temperature convert 4h, and 250 DEG C of constant temperature convert 4h, and 280 DEG C of constant temperature convert 5h, and 325 DEG C of constant temperature convert 5h, and 370 DEG C
Constant temperature converts 8h, and 390 DEG C of constant temperature convert 18h.
It further, further include normal through the step (V) by the production technology that depth pickling yellow phosphorus is converted into electronic grade red phosphorus
The step of converted product is dried in vacuo after the step of super pressure-high temperature converts, and its drying temperature is 160~170 DEG C, drying time 3
~5h.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention is by improving traditional industry grade yellow phosphorus acid cleaning process, will be diluted to after mass fraction is 20%
It is added to continued mechanical in the enamel cast iron kettle for install industrial yellow phosphorus to stir, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitre
It is cleaned with pure water by relatively mild with mechanical deep stirring replacement tradition after impurity sufficiently reacts in the sour and described industrial yellow phosphorus
Air agitation, come into full contact with yellow phosphorus and nitric acid, remove the impurity that the subsequent techniques such as S, C and As not can be removed, greatly improve
Product purity.
2. the present invention is converted into electronic grade red phosphorus by depth pickling yellow phosphorus, the yellow phosphorus rate of recovery is greatly improved, and increases red phosphorus
Yield, and reaction process be not necessarily to additive, reduce production cost.
3. in depth acid cleaning process of the present invention, replacing traditional quartz reaction using the interior enamel cast iron kettle with outside sandwich
Kettle substantially reduces production safety hidden danger.
Specific embodiment
Below with reference to embodiment, the present invention is further described.
Embodiment 1
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, method particularly includes:
(1) depth pickling: it is 20% that the nitric acid that mass fraction is 68%, which is diluted to mass fraction, is added to and installs industry
Continued mechanical stirs in the enamel cast iron kettle of yellow phosphorus, and kettle outside sandwich recycles logical hot water thermal insulating, makes in nitric acid and industrial yellow phosphorus
Impurity including As, S and C sufficiently reacts, then reaction product is cleaned with pure water, and the mass ratio of nitric acid and industrial yellow phosphorus is 1:3.
(2) chlorination: the yellow phosphorus after depth pickling is transferred in chlorination tank, is passed through chlorine and is reacted generation tri-chlorination with yellow phosphorus
The mass ratio of phosphorus, chlorine and yellow phosphorus is 1:0.29.
(3) rectifying: temperature is different by not having to component volatilization degree 20 DEG C more than phosphorus trichloride boiling point in control rectifying column
While separating impurity, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment, repeats above-mentioned rectifying
Journey 3 times.
(4) it hydrogen reducing: is passed through in the reaction tube of the phosphorus trichloride obtained equipped with rectifying and is reacted with 5N hydrogen, obtained
6N yellow phosphorus.
(5) constant-pressure and high-temperature converts: the 6N yellow phosphorus that reduction is obtained is packed into conversion tube, and to 400 DEG C, conversion obtains ladder-elevating temperature
The electronic grade red phosphorus that purity is 99.9999% obtains 6N red phosphorus product through 160 DEG C of vacuum drying 3h.Wherein, ladder-elevating temperature process
Are as follows: 180 DEG C of constant temperature convert 3h, and 200 DEG C of constant temperature convert 3h, and 220 DEG C of constant temperature convert 3h, and 240 DEG C of constant temperature convert 3h, 260 DEG C of constant temperature
3h is converted, 300 DEG C of constant temperature convert 3h, and 350 DEG C of constant temperature convert 6h, and 380 DEG C of constant temperature convert 12h.
Embodiment 2
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, method particularly includes:
(1) it depth pickling: the nitric acid that mass fraction is 68% is diluted to be added to after mass fraction is 20% installs work
In the enamel cast iron kettle of industry yellow phosphorus, and continued mechanical stirring is carried out, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and work
Impurity in industry yellow phosphorus including As, S and C sufficiently reacts, then reaction product is cleaned with pure water, the quality of nitric acid and industrial yellow phosphorus
Than for 1:3.
(2) chlorination: the yellow phosphorus after depth pickling is transferred in chlorination tank, is passed through chlorine and is reacted generation tri-chlorination with yellow phosphorus
The mass ratio of phosphorus, chlorine and yellow phosphorus is 1:0.29.
(3) rectifying: temperature is different by not having to component volatilization degree 30 DEG C more than phosphorus trichloride boiling point in control rectifying column
While separating impurity, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment, repeats above-mentioned rectifying
Journey 5 times.
(4) it hydrogen reducing: is passed through in the reaction tube of the phosphorus trichloride obtained equipped with rectifying and is reacted with 5N hydrogen, obtained
6N yellow phosphorus.
(5) constant-pressure and high-temperature converts: the 6N yellow phosphorus that reduction is obtained is packed into conversion tube, and to 400 DEG C, conversion obtains ladder-elevating temperature
The electronic grade red phosphorus that purity is 99.9999% obtains 6N red phosphorus product through 170 DEG C of vacuum drying 5h.Wherein, ladder-elevating temperature process
Are as follows: 200 DEG C of constant temperature convert 6h, and 220 DEG C of constant temperature convert 6h, and 240 DEG C of constant temperature convert 6h, and 260 DEG C of constant temperature convert 6h, 300 DEG C of constant temperature
6h is converted, 350 DEG C of constant temperature convert 6h, and 380 DEG C of constant temperature convert 12h, and 400 DEG C of constant temperature conversions are for 24 hours.
Embodiment 3
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, method particularly includes:
(1) it depth pickling: the nitric acid that mass fraction is 68% is diluted to be added to after mass fraction is 20% installs work
In the enamel cast iron kettle of industry yellow phosphorus, and continued mechanical stirring is carried out, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and work
Impurity in industry yellow phosphorus including As, S and C sufficiently reacts, then reaction product is cleaned with pure water, the quality of nitric acid and industrial yellow phosphorus
Than for 1:3.
(2) chlorination: the yellow phosphorus after depth pickling is transferred in chlorination tank, is passed through chlorine and is reacted generation tri-chlorination with yellow phosphorus
The mass ratio of phosphorus, chlorine and yellow phosphorus is 1:0.29.
(3) rectifying: temperature is different by not having to component volatilization degree 25 DEG C more than phosphorus trichloride boiling point in control rectifying column
While separating impurity, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment, repeats above-mentioned rectifying
Journey 3 times.
(4) it hydrogen reducing: is passed through in the reaction tube of the phosphorus trichloride obtained equipped with rectifying and is reacted with 5N hydrogen, obtained
6N yellow phosphorus.
(5) constant-pressure and high-temperature converts: the 6N yellow phosphorus that reduction is obtained is packed into conversion tube, and to 400 DEG C, conversion obtains ladder-elevating temperature
The electronic grade red phosphorus that purity is 99.9999% obtains 6N red phosphorus product through 165 DEG C of vacuum drying 4h.Wherein, ladder-elevating temperature process
Are as follows: 185 DEG C of constant temperature convert 5h, and 205 DEG C of constant temperature convert 5h, and 225 DEG C of constant temperature convert 5h, and 245 DEG C of constant temperature convert 5h, 275 DEG C of constant temperature
5h is converted, 315 DEG C of constant temperature convert 5h, and 365 DEG C of constant temperature convert 12h, and 385 DEG C of constant temperature conversions are for 24 hours.
Embodiment 4
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, method particularly includes:
(1) it depth pickling: the nitric acid that mass fraction is 68% is diluted to be added to after mass fraction is 20% installs work
In the enamel cast iron kettle of industry yellow phosphorus, and continued mechanical stirring is carried out, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and work
Impurity in industry yellow phosphorus including As, S and C sufficiently reacts, then reaction product is cleaned with pure water, the quality of nitric acid and industrial yellow phosphorus
Than for 1:3.
(2) chlorination: the yellow phosphorus after depth pickling is transferred in chlorination tank, is passed through chlorine and is reacted generation tri-chlorination with yellow phosphorus
The mass ratio of phosphorus, chlorine and yellow phosphorus is 1:0.29.
(3) rectifying: temperature is different by not having to component volatilization degree 20 DEG C more than phosphorus trichloride boiling point in control rectifying column
While separating impurity, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment, repeats above-mentioned rectifying
Journey 4 times.
(4) it hydrogen reducing: is passed through in the reaction tube of the phosphorus trichloride obtained equipped with rectifying and is reacted with 5N hydrogen, obtained
6N yellow phosphorus.
(5) constant-pressure and high-temperature converts: the 6N yellow phosphorus that reduction is obtained is packed into conversion tube, and to 400 DEG C, conversion obtains ladder-elevating temperature
The electronic grade red phosphorus that purity is 99.9999% obtains 6N red phosphorus product through 168 DEG C of vacuum drying 5h.Wherein, ladder-elevating temperature process
Are as follows: 195 DEG C of constant temperature convert 3h, and 215 DEG C of constant temperature convert 3h, and 235 DEG C of constant temperature convert 3h, and 255 DEG C of constant temperature convert 3h, 285 DEG C of constant temperature
3h is converted, 335 DEG C of constant temperature convert 3h, and 375 DEG C of constant temperature convert 8h, and 395 DEG C of constant temperature convert 16h.
Embodiment 5
The production technology of electronic grade red phosphorus is converted by depth pickling yellow phosphorus, method particularly includes:
(1) it depth pickling: the nitric acid that mass fraction is 68% is diluted to be added to after mass fraction is 20% installs work
In the enamel cast iron kettle of industry yellow phosphorus, and continued mechanical stirring is carried out, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and work
Impurity in industry yellow phosphorus including As, S and C sufficiently reacts, then reaction product is cleaned with pure water, the quality of nitric acid and industrial yellow phosphorus
Than for 1:3.
(2) chlorination: the yellow phosphorus after depth pickling is transferred in chlorination tank, is passed through chlorine and is reacted generation tri-chlorination with yellow phosphorus
The mass ratio of phosphorus, chlorine and yellow phosphorus is 1:0.29.
(3) rectifying: temperature is different by not having to component volatilization degree 30 DEG C more than phosphorus trichloride boiling point in control rectifying column
While separating impurity, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment, repeats above-mentioned rectifying
Journey 4 times.
(4) it hydrogen reducing: is passed through in the reaction tube of the phosphorus trichloride obtained equipped with rectifying and is reacted with 5N hydrogen, obtained
6N yellow phosphorus.
(5) constant-pressure and high-temperature converts: the 6N yellow phosphorus that reduction is obtained is packed into conversion tube, and to 400 DEG C, conversion obtains ladder-elevating temperature
The electronic grade red phosphorus that purity is 99.9999% obtains 6N red phosphorus product through 162 DEG C of vacuum drying 5h.Wherein, ladder-elevating temperature process
Are as follows: 190 DEG C of constant temperature convert 4h, and 210 DEG C of constant temperature convert 4h, and 230 DEG C of constant temperature convert 4h, and 250 DEG C of constant temperature convert 4h, 280 DEG C of constant temperature
5h is converted, 325 DEG C of constant temperature convert 5h, and 370 DEG C of constant temperature convert 8h, and 390 DEG C of constant temperature convert 18h.
After tested, the electron level of the production technology preparation of electronic grade red phosphorus is converted by depth pickling yellow phosphorus through the invention
Impurity content is as shown in table 1 below in red phosphorus.
Table 1 (unit: PPM)
Claims (10)
1. being converted into the production technology of electronic grade red phosphorus by depth pickling yellow phosphorus, which is characterized in that by industrial yellow phosphorus successively through wrapping
It includes
(I) depth pickling, and
(II) chlorination, and
(III) rectifying, and
(IV) hydrogen reducing, and
The step of (V) constant-pressure and high-temperature converts obtains the electronic grade red phosphorus that purity is 99.9999%；Wherein:
In step (I), the depth pickling process includes: that will be diluted to the nitric acid that mass fraction is 20% to be added to and install industry
Continued mechanical intense agitation is carried out in the enamel cast iron kettle of yellow phosphorus, and kettle outside sandwich recycles logical hot water thermal insulating, makes nitric acid and institute
It states impurity in industrial yellow phosphorus sufficiently to react, then reaction product is cleaned with pure water；Wherein, the impurity includes As, S and C, described
The mass ratio of nitric acid and industrial yellow phosphorus is 1:3.
2. the production technology of electronic grade red phosphorus according to claim 1, which is characterized in that in step (II), the chlorination work
Sequence are as follows: the yellow phosphorus after depth pickling in step (I) is transferred in chlorination tank, chlorine is passed through and reacts generation tri-chlorination with yellow phosphorus
Phosphorus, the phosphorus trichloride volatilization generated in the case where reacting heat effect, collects liquid phosphorus trichloride after condensation segment；Wherein, the chlorine
Mass ratio with yellow phosphorus is 1:0.29.
3. the production technology of electronic grade red phosphorus according to claim 1, which is characterized in that in step (III), the rectifying work
Sequence are as follows: temperature separates the same of impurity by not having to component volatilization degree difference more than the boiling point of phosphorus trichloride in control rectifying column
When, the steam of phosphorus trichloride becomes liquids recovery after rising to rectifying column condensation segment；It repeats above-mentioned distillation process 3~5 times.
4. the production technology of electronic grade red phosphorus according to claim 3, which is characterized in that in step (III), the rectifying column
20~30 DEG C more than phosphorus trichloride boiling point, steam rises to after the condensation segment of rectifying column to be become liquid and returns the control of interior temperature
It receives, repeats above-mentioned distillation process 3~4 times.
5. the production technology of electronic grade red phosphorus according to claim 4, which is characterized in that in step (III), the rectifying column
20~25 DEG C more than phosphorus trichloride boiling point, steam rises to after the condensation segment of rectifying column to be become liquid and returns the control of interior temperature
It receives, repeats above-mentioned distillation process 4 times.
6. the production technology of electronic grade red phosphorus according to claim 1, which is characterized in that in step (IV), the hydrogen is also
Former process are as follows: be passed through in the reaction tube of the phosphorus trichloride obtained equipped with step (III) rectifying and reacted with 5N hydrogen, obtain 6N
Yellow phosphorus.
7. the production technology of electronic grade red phosphorus according to claim 1, which is characterized in that in step (V), the normal pressure is high
Warm conversion procedure are as follows: the 6N yellow phosphorus that reduction obtains in step (IV) is packed into conversion tube, to 400 DEG C, conversion obtains ladder-elevating temperature
6N red phosphorus；Wherein:
The ladder-elevating temperature process are as follows: 180~200 DEG C of constant temperature convert 3~6h, and 200~220 DEG C of constant temperature convert 3~6h, 220~
240 DEG C of constant temperature convert 3~6h, and 240~260 DEG C of constant temperature convert 3~6h, and 260~300 DEG C of constant temperature convert 3~6h, and 300~350 DEG C
Constant temperature converts 3~6h, and 350~380 DEG C of constant temperature convert 6~12h, and 380~400 DEG C of constant temperature conversions 12~for 24 hours.
8. the production technology of electronic grade red phosphorus according to claim 7, which is characterized in that in step (V), the ladder liter
Warm conversion process are as follows: 185~195 DEG C of constant temperature convert 3~5h, and 205~215 DEG C of constant temperature convert 3~5h, 225~235 DEG C of constant temperature rotaries
Change 3~5h, 245~255 DEG C of constant temperature convert 3~5h, and 275~285 DEG C of constant temperature convert 3~5h, 315~335 DEG C of constant temperature conversions 3~
5h, 365~375 DEG C of 8~12h of constant temperature conversion, 385~395 DEG C of constant temperature conversions 16~for 24 hours.
9. according to the production technology of the electronic grade red phosphorus of claim 7 or 8, which is characterized in that in step (V), the ladder
Heat up conversion process are as follows: 190 DEG C of constant temperature convert 4h, and 210 DEG C of constant temperature convert 4h, and 230 DEG C of constant temperature convert 4h, 250 DEG C of constant temperature conversions
4h, 280 DEG C of constant temperature convert 5h, and 325 DEG C of constant temperature convert 5h, and 370 DEG C of constant temperature convert 8h, and 390 DEG C of constant temperature convert 18h.
10. the production technology of electronic grade red phosphorus according to claim 1, which is characterized in that any one of claim 1~9 institute
The production technology for stating electronic grade red phosphorus further includes the steps that converted product vacuum is dry after the step (V) constant-pressure and high-temperature converts
Dry step, and its drying temperature is 160~170 DEG C, drying time is 3~5h.
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