CN103086333A - Production technique of red phosphorus by means of high temperature sealing method - Google Patents
Production technique of red phosphorus by means of high temperature sealing method Download PDFInfo
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- CN103086333A CN103086333A CN2013100140002A CN201310014000A CN103086333A CN 103086333 A CN103086333 A CN 103086333A CN 2013100140002 A CN2013100140002 A CN 2013100140002A CN 201310014000 A CN201310014000 A CN 201310014000A CN 103086333 A CN103086333 A CN 103086333A
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Abstract
The invention provides a production technique of red phosphorus by means of a high temperature sealing method. The production technique specifically comprises the following steps of: (1) adding yellow phosphorus into a phosphorus dissolving tank, transferring the dissolved yellow phosphorus into conversion kettles in batch after the yellow phosphorus is dissolved, and sealing the conversion kettles; (2) directly placing the conversion kettles into a plurality of conversion electric furnaces which are distributed in a rectangular array to form a conversion electric furnace group functioning as equipment, under the condition of insulating air, converting the yellow phosphorus for 60-74 hours, cooling the converted product and discharging the cooled product to obtain a red phosphorus semi-finished product; (3) crushing the red phosphorus semi-finished product by a crushing machine; (4) conveying the crushed red phosphorus semi-finished product into a soda boiling head tank by a plugging-free mechanical pump, and then conveying slurry from the soda boiling head tank to a soda boiling kettle for soda boiling reaction; and (5) cleaning, dehydrating and dying the resulting product to obtain a red phosphorus finished product. When the method provided by the invention is applied to the red phosphorus production, the production safety can be ensured, impurities in the product can be reduced, the product quality and the production efficiency are improved, the labor intensity of an operator is reduced, and the product processing cost is reduced.
Description
Technical field
The present invention relates to produce the processing method of red phosphorus, especially the high-temperature closed method is produced the processing method of red phosphorus.
Background technology
At present, produce red phosphorus technical process be: yellow phosphorus → dress pot fusing → pyrolytic conversion → ball milling → soda boiling → cleaning → centrifugal dewatering → vacuum drying → packing is put in storage.Transforming principle is: with the yellow phosphorus that installs in the situation that isolated air, the long-time heating temperature is 295 ℃ of-300 ℃ of left and right, can transfer red phosphorus to, through abrasive material, after the soda boiling reaction, after cleaning, dewater, drying, the finished product red phosphorus that obtains, whole red phosphorus production technique is comprised of operations such as conversion, ball milling, soda boiling, washing, dehydration post-drying packings.
Existing produce red phosphorus technique be: in transforming pot after fusing, directly lift up into and transform in electric furnace transforming pot integral body, cover bell, power transmission transforms, complete through conversion in 72 hours after, hang out converter; Then, add the water wet-milling with ball mill, carry out conveying to the soda boiling header tank, slip is delivered in the soda boiling pot, under agitation with the sodium hydroxide solution that slowly adds 60% after steam indirect heating to 50 ℃, removed a small amount of yellow phosphorus with this, generally through 2.5 hours, make the pH value reach 8-8.5; After soda boiling is complete, slip is put into rinse bath washing, then through dehydration, oven dry, packing.
The problem that existing technique exists:
1. direct fusion in transforming pot after will waiting for a plurality of yellow phosphorus fusings that transform in pot, then hangs in to transform in the electric furnace group and transforms, in melting process, and the artificial yellow phosphorus that directly contacts, dangerous, labour intensity is large, loses time;
2. with the ball mill ball milling time, operator's material loading, blanking labour intensity is larger, inconvenient operation, because milling time is long, the slurry iron-holder that grinds is high, and impurity is more;
3. when carrying out conveying to the soda boiling header tank, adopt the binder tank to add the mode of compressed gas, easily clog during binder, misoperation easily causes security incident, takies equipment more;
4. centrifugal dewatering, noise is large, and labour intensity is higher, and production environment is poor.
Summary of the invention
In order to improve the quality of products and production efficiency, reduce labour intensity, reduce the tooling cost of product, the present invention proposes the processing method that the high-temperature closed method is produced red phosphorus.
For achieving the goal, the present invention by the following technical solutions: the high-temperature closed method is produced the processing method of red phosphorus, and concrete steps are as follows:
(1). the yellow phosphorus fusing: yellow phosphorus is put into molten phosphorus groove, adopt electric heating tube to heat, after yellow phosphorus dissolves well, be encased in batches in the conversion pot, sealing conversion pot, every batch will fill the 5-10 pot; The volumetric ratio of described molten phosphorus groove transforms the large 4-9 of volume times of pot;
(2). pyrolytic conversion: the conversion electric furnace group that adopts the rectangular arranged in arrays of a plurality of conversion electric furnaces to consist of is equipment; Conversion electric furnace between every two row consists of one group, and the conversion electric furnace between every group of two row shares a tank, and the conversion electric furnace between every group of two row shares a smoking pipeline;
Directly a plurality of conversion pots that yellow phosphorus is housed are put into respectively a plurality of conversion electric furnaces, then heat up, in the situation that isolated air guarantees to transform the interior temperature of electric furnace at 280 ℃-300 ℃, transformation time was at 60-74 hour; Then, hang out converter transforming pot, be cooled to below 50 ℃, then discharging gets the red phosphorus work in-process;
(3). pulverize: adopt pulverizer to carry out wet pulverization to the red phosphorus work in-process, get slip;
(4). soda boiling: with carrying out conveying without stopping up mechanical pump to the soda boiling header tank, then slip to the soda boiling pot, carries out the soda boiling reaction from the soda boiling header tank slip;
(5). clean: water carries out rinsing;
(6). dehydration: adopt filter pocket to anhydrate by vacuum filtration;
(7). oven dry: adopt the vacuum drying oven oven dry, the red phosphorus finished product.
Beneficial effect: the present invention has reduced labour intensity by concentrating molten phosphorus, enhances productivity, and has guaranteed production safety; By transforming the rational deployment of electric furnace group, reduce energy consumption, guarantee that smoke evacuation is unobstructed; Substitute ball mill by pulverizer and pulverize, reduced labour intensity, reduced grinding time, avoid to greatest extent the generation of impurity, guarantee quality product; Adopt the non-blocked mechanical pump to carry out conveying, easy to operate, delivery rate is fast, do not stop up, and safety; Adopt vacuum filtration to substitute centrifuge, can concentrate blowing, stop to throw, spill, leak phenomenon, labour intensity reduces, the work-yard environmental improvement.Summary adopts method of the present invention to produce red phosphorus, can guarantee production safety, can improve the quality of products and production efficiency than the impurity in low production, reduces labor intensity of operating staff, reduces the tooling cost of product.
Description of drawings
Fig. 1 transforms the arrangement figure of electric furnace group in the present invention.
Embodiment
The present invention adjusts (comprising equipment, process procedure bridging mode etc.) to the process procedure of high-temperature closed method production red phosphorus, do not relate to the adjustment to the auxiliary material that uses in starting material and process procedure, the auxiliary material that uses in starting material and process procedure is consistent with prior art.
Below, further describe the present invention with an embodiment as follows.
The high-temperature closed method is produced the processing method of red phosphorus, and concrete steps are as follows:
(1). the yellow phosphorus fusing: yellow phosphorus is put into molten phosphorus groove, adopt electric heating tube to heat, after yellow phosphorus dissolves well, be encased in batches in the conversion pot, sealing conversion pot, every batch will fill 5 pots; Large 4 times of the volume of the volumetric ratio conversion pot of described molten phosphorus groove;
(2). pyrolytic conversion: the conversion electric furnace group that adopts the rectangular arranged in arrays of a plurality of conversion electric furnaces to consist of is equipment, as shown in Figure 1, conversion electric furnace 1 between every two row consists of one group, shown in Fig. 1 be 2 groups, conversion electric furnace 1 between every group of two row shares a tank 2, and the conversion electric furnace between every group of two row shares a smoking pipeline 3; 2 groups transform between electric furnace is walking passage 4;
Directly a plurality of conversion pots that yellow phosphorus is housed are put into respectively a plurality of conversion electric furnaces 1, then heat up, in the situation that isolated air guarantees to transform the interior temperature of electric furnace at 280 ℃-300 ℃, transformation time was at 72 hours; Then, hang out converter transforming pot, be cooled to below 50 ℃, then discharging gets the red phosphorus work in-process;
Wherein, the thermal insulation layer of described conversion electric furnace is the perlite packing layer;
(3). pulverize: adopt pulverizer to carry out wet pulverization to the red phosphorus work in-process, get slip;
(4). soda boiling: with carrying out conveying without stopping up mechanical pump to the soda boiling header tank, then slip to the soda boiling pot, carries out the soda boiling reaction from the soda boiling header tank slip;
(5). clean: water carries out rinsing;
(6). dehydration: adopt filter pocket to anhydrate by vacuum filtration;
(7). oven dry: adopt the vacuum drying oven oven dry, the red phosphorus finished product.
At last, the red phosphorus finished product packing is put in storage.
In above-described embodiment, every batch will fill 5 pots, large 4 times of the volume of the volumetric ratio conversion pot of described molten phosphorus groove; In actual production, according to industrial scale, every batch can be adjusted between the 5-10 pot, and the volumetric ratio of described molten phosphorus groove transforms the large 4-9 of volume times of pot.
In above-described embodiment, the pyrolytic conversion time is 72 hours.In actual production, the pyrolytic conversion time can be adjusted between 60-74 hour.
In above-described embodiment, soda boiling reaction and cleaning step are consistent with prior art, and auxiliary material used is also consistent, is not described in detail at this.
In above-described embodiment, the thermal insulation layer that transforms electric furnace is the perlite packing layer, and better heat preservation can reduce energy consumption.
In above-described embodiment, transform scale and the group number of electric furnace group, have industrial scale to determine, be not limited to 2 groups; Transform the electric furnace group as long as adopt the rectangular arranged in arrays of a plurality of conversion electric furnaces to consist of, can achieve the goal.
The present invention compared with prior art, advantage is as follows:
1. will be improved to and concentrate molten phosphorus or fill pot in batches originally carrying out molten phosphorus in transforming pot, the firstth, reduce labor intensity, to boost productivity, the second safety coefficient significantly improves;
2. improve the arrangement that transforms the electric furnace group, be improved to two stoves by original both sides tank and share one, be improved to intermediate conduit by original both sides smoke evacuation and concentrate mechanical forced fume exhaust, smoke discharging effect is good, has also reduced energy consumption; The thermal insulation layer of described conversion electric furnace adopts the perlite packing layer, can further reduce energy consumption;
3. substitute ball mill by pulverizer and pulverize, reduced labour intensity, reduced grinding time, avoid to greatest extent the generation of impurity, guarantee quality product;
4. adopt the non-blocked mechanical pump to carry out conveying, easy to operate, delivery rate is fast, do not stop up, and safety;
5. adopt vacuum filtration to substitute centrifuge, can concentrate blowing, stop to throw, spill, leak phenomenon, labour intensity reduces, the work-yard environmental improvement.
Claims (1)
1. the high-temperature closed method is produced the processing method of red phosphorus, and concrete steps are as follows:
(1). the yellow phosphorus fusing: yellow phosphorus is put into molten phosphorus groove, adopt electric heating tube to heat, after yellow phosphorus dissolves well, be encased in batches in the conversion pot, sealing conversion pot, every batch will fill the 5-10 pot; The volumetric ratio of described molten phosphorus groove transforms the large 4-9 of volume times of pot;
(2). pyrolytic conversion: the conversion electric furnace group that adopts the rectangular arranged in arrays of a plurality of conversion electric furnaces to consist of is equipment; Conversion electric furnace between every two row consists of one group, and the conversion electric furnace between every group of two row shares a tank, and the conversion electric furnace between every group of two row shares a smoking pipeline;
Directly a plurality of conversion pots that yellow phosphorus is housed are put into respectively a plurality of conversion electric furnaces, then heat up, in the situation that isolated air guarantees to transform the interior temperature of electric furnace at 280 ℃-300 ℃, transformation time was at 60-74 hour; Then, hang out converter transforming pot, be cooled to below 50 ℃, then discharging gets the red phosphorus work in-process;
(3). pulverize: adopt pulverizer to carry out wet pulverization to the red phosphorus work in-process, get slip;
(4). soda boiling: with carrying out conveying without stopping up mechanical pump to the soda boiling header tank, then slip to the soda boiling pot, carries out the soda boiling reaction from the soda boiling header tank slip;
(5). clean: water carries out rinsing;
(6). dehydration: adopt filter pocket to anhydrate by vacuum filtration;
(7). oven dry: adopt the vacuum drying oven oven dry, the red phosphorus finished product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013100140002A CN103086333A (en) | 2013-01-15 | 2013-01-15 | Production technique of red phosphorus by means of high temperature sealing method |
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| CN2013100140002A CN103086333A (en) | 2013-01-15 | 2013-01-15 | Production technique of red phosphorus by means of high temperature sealing method |
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| CN103086333A true CN103086333A (en) | 2013-05-08 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108529579A (en) * | 2018-04-26 | 2018-09-14 | 山东亿盛实业股份有限公司 | A kind of method that ultrasound adverse current refines red phosphorus crude product |
| CN109081320A (en) * | 2018-10-16 | 2018-12-25 | 贵阳精科技有限公司 | A kind of electronic grade high-purity yellow phosphorus is converted into the device and method of red phosphorus |
| CN110790247A (en) * | 2019-12-16 | 2020-02-14 | 湖北尧治河化工股份有限公司 | New process for producing red phosphorus by using yellow phosphorus |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556988A (en) * | 2011-12-23 | 2012-07-11 | 东方电气集团峨嵋半导体材料有限公司 | Ultra-pure white phosphorus ordinary-pressure conversion method |
-
2013
- 2013-01-15 CN CN2013100140002A patent/CN103086333A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102556988A (en) * | 2011-12-23 | 2012-07-11 | 东方电气集团峨嵋半导体材料有限公司 | Ultra-pure white phosphorus ordinary-pressure conversion method |
Non-Patent Citations (1)
| Title |
|---|
| 李金福: "我省发展赤磷生产的可行性初探", 《贵州化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108529579A (en) * | 2018-04-26 | 2018-09-14 | 山东亿盛实业股份有限公司 | A kind of method that ultrasound adverse current refines red phosphorus crude product |
| CN109081320A (en) * | 2018-10-16 | 2018-12-25 | 贵阳精科技有限公司 | A kind of electronic grade high-purity yellow phosphorus is converted into the device and method of red phosphorus |
| CN110790247A (en) * | 2019-12-16 | 2020-02-14 | 湖北尧治河化工股份有限公司 | New process for producing red phosphorus by using yellow phosphorus |
| CN110790247B (en) * | 2019-12-16 | 2021-10-08 | 湖北尧治河化工股份有限公司 | Process for producing red phosphorus by using yellow phosphorus |
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Application publication date: 20130508 |