CN107601446B - Device and method for continuously recovering yellow phosphorus in phosphorus mud through multistage evaporation - Google Patents

Device and method for continuously recovering yellow phosphorus in phosphorus mud through multistage evaporation Download PDF

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CN107601446B
CN107601446B CN201710995305.4A CN201710995305A CN107601446B CN 107601446 B CN107601446 B CN 107601446B CN 201710995305 A CN201710995305 A CN 201710995305A CN 107601446 B CN107601446 B CN 107601446B
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phosphorus
dryer
mud
paddle
paddle dryer
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CN107601446A (en
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夏志华
聂兴臻
张朝坤
万源
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Hubei Jixing Chemical Industry Group Corporation Limited
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HUBEI JIXING CHEMICAL INDUSTRY GROUP Corp Ltd
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Abstract

The invention provides a device for recovering yellow phosphorus in phosphorus mud through continuous multi-stage evaporation, wherein the phosphorus mud enters a pipeline and is connected with a screw stacking machine, the screw stacking machine is connected with a first blade dryer through a first screw feeder, and the first blade dryer is connected with a second blade dryer; the heat conduction oil pipeline and the heat medium storage tank are connected with a gas boiler through a hot oil pump, and the gas boiler is respectively connected with the bottoms of the first paddle dryer and the second paddle dryer; the tops of the first paddle dryer and the second paddle dryer are respectively connected with the washing tower trough through pipelines. Yellow phosphorus is evaporated from phosphorus mud by using an evaporation principle, the yellow phosphorus is recovered, the phosphorus mud enters a primary paddle dryer from a discharge hole of a storage tank by a screw conveyor to evaporate water, then enters a secondary paddle dryer to evaporate the yellow phosphorus, and heat is provided for the dryer by a heat medium fluid. The method for recovering the yellow phosphorus in the phosphorus mud by continuous multi-stage evaporation can efficiently recover the element phosphorus in the phosphorus mud, the whole process equipment is well sealed, no obvious smoke exists on the site, the quality of the recovered yellow phosphorus is excellent, and the recovered residue can be naturally stacked.

Description

Device and method for continuously recovering yellow phosphorus in phosphorus mud through multistage evaporation
Technical Field
The invention relates to a method and a device for recovering yellow phosphorus in phosphorus mud through continuous multi-stage evaporation, belonging to the field of chemical equipment and chemical production.
Background
The existing methods for recovering the phosphorus mud can be divided into a phosphorus mud acid burning method, a physical separation method and a chemical separation method.
The phosphoric mud acid burning method is to burn phosphoric mud directly, and phosphorus pentoxide generated by the combustion of yellow phosphorus is absorbed in a hydration absorption tower to become phosphoric acid. The equipment of the method comprises an incinerator and an absorption device.
The physical separation mainly comprises extraction, filtration and phosphorus steaming separation, and mainly comprises extraction equipment, a filter or a phosphorus steaming pot. Although phosphorus evaporation is simple, equipment corrosion is large, the field environment is poor, and the residue contains a small amount of elemental phosphorus.
The chemical separation method mainly comprises the following steps: hydrochloric acid-nitric acid method, soda method, ammonolysis method, ammonium carbonate-caustic soda-hydrogen peroxide method. At present, the methods generally carry out the reaction in a reaction kettle, and the phosphorus is discharged from the bottom after the reaction is finished, so the method has simple structure but is inconvenient to operate, and the phosphorus pentoxide gas generated by the reaction is not absorbed and is discharged into the atmosphere, so the operating environment is quite severe.
The invention provides a method and equipment for evaporating and recovering yellow phosphorus in phosphorus mud, and the method has the advantages of high recovery rate, no smoke on site, good environment, harmless residues and simple and convenient operation.
Disclosure of Invention
The invention provides a method and a device for continuously evaporating and recovering yellow phosphorus in phosphorus mud in multiple stages, which evaporate yellow phosphorus from phosphorus mud by using an evaporation principle so as to achieve the aim of recovering the yellow phosphorus. The method comprises the following specific steps:
the device for recovering yellow phosphorus in phosphorus mud through continuous multi-stage evaporation comprises a phosphorus mud inlet pipeline, a screw stacking machine, a screw feeder I, a blade dryer II and a screw evaporator I, wherein the phosphorus mud inlet pipeline is connected with the screw stacking machine;
the heat conducting oil pipeline and the heat medium storage tank are connected with a gas boiler through a hot oil pump, the gas boiler is respectively connected with the bottoms of the first paddle dryer and the second paddle dryer, and the tops of the first paddle dryer and the second paddle dryer are respectively converged with a pipeline from the gas boiler through pipelines and then connected with the heat medium storage tank;
the tops of the first paddle dryer and the second paddle dryer are respectively connected with the washing tower trough through pipelines.
The gas inlet pipeline outside the boundary area is connected with a gas boiler, and the gas boiler is connected with a chimney; the external clean water pipeline is connected with the upper part of the washing tower groove, the external steam pipeline is connected with the lower part of the washing tower groove, and the top of the washing tower groove is connected with the chimney; the upper part of the washing tower tank is connected with a yellow phosphorus sewage pool outside the overflow boundary area, and the lower part of the washing tower tank is connected with a condensed water discharge pipe.
And nitrogen introducing pipelines are arranged at the tops of the screw feeder, the first paddle dryer and the second paddle dryer.
And the bottom of the second paddle dryer is connected to the waste residue bin through a second screw feeder.
The spiral shell stacking machine is connected with a yellow phosphorus sewage pool outside the overflow boundary area.
The device for continuously and multistage evaporating and recovering the yellow phosphorus in the phosphorus mud is used for evaporating element phosphorus from the phosphorus mud by using an evaporation principle so as to achieve the purpose of recovering the yellow phosphorus, the phosphorus mud is dehydrated by dehydration equipment and then transferred into a phosphorus mud storage tank, the phosphorus mud enters a primary paddle dryer from a discharge port of the storage tank by a screw feeder to evaporate water, automatically flows into a secondary paddle dryer through a slag outlet of the primary paddle dryer to evaporate the element phosphorus, a star-shaped feeder is arranged at the slag outlet of the secondary paddle dryer to discharge slag, and the evaporated residue can be directly buried or processed into a compound fertilizer by a fertilizer factory; the heating medium is heated by the heating device, flows into the primary paddle dryer through the centrifugal pump and the secondary paddle dryer, and returns to the heating medium storage tank for recycling; and the evaporated gas of the primary paddle dryer and the secondary paddle dryer enters a washing tower tank to be condensed to recover water vapor and yellow phosphorus.
The drying temperature of the phosphorus mud passing through the primary blade dryer is 110-350 ℃, and the drying temperature of the secondary blade dryer is 280-350 ℃. The paddle dryer is hollow, the heat medium fluid is used for indirectly heating the phosphorus mud, the three-stage sealing is respectively used for sealing two ends of the paddle by the filler, the inert gas and the filler, so that the contact of air and the phosphorus mud is avoided, the heat medium fluid two-stage hollow paddle dryer flows into the one-stage hollow paddle dryer, and the two-stage heat sources are connected in series for use. The phosphorus mud stays in the first-stage hollow blade dryer for 2-4 hours, and stays in the second-stage hollow blade dryer for 3-8 hours. The heat medium fluid can be heat conducting oil and steam.
The invention can change the phosphorus mud into valuable, and efficiently recover the element phosphorus in the phosphorus mud, and because the yellow phosphorus is recovered by low-temperature evaporation, the yellow phosphorus has high purity and low arsenic content; the residue contains a small amount of phosphate which can be used as a raw material of a compound fertilizer; the evaporated water is condensed and recovered to be used as yellow phosphorus spray water, so that the comprehensive recycling is realized, and three wastes are not generated. The tail gas generated in the production of yellow phosphorus is used as a heat source, the phosphorus mud is dehydrated by the screw stacking machine and then enters the blade dryer, the water content of the phosphorus mud is low, and the heat conducting oil is used as a circulating heat carrier, so that the heat energy is fully utilized, the consumption of the tail gas of the yellow phosphorus is reduced, and the energy is saved. The production equipment fully considers the sealing property and isolates air, avoids the leakage and leakage of the phosphorus mud in the production field and the spontaneous combustion of the phosphorus mud, and achieves good environment of the production field and inorganization smoke emission. The production process has high degree of mechanization and greatly reduces the labor intensity.
Drawings
The invention is further illustrated by the following figures and examples.
Figure 1 is a process flow diagram.
Detailed Description
The method comprises the following operation steps:
1. pretreating phosphorus mud: the phosphorus mud is pumped into a screw stacking machine by a mud pump to be partially dehydrated and then transferred into a phosphorus mud storage tank.
2. And (2) starting the two dryers, adjusting the rotating speed to be 2-8 r/min, replacing gas in the two dryers with inert gas, wherein the oxygen content is lower than 5%, starting heat conducting oil, and starting a phosphorus mud feeding screw conveyor (or a screw pump) when the temperature in the primary hollow blade dryer reaches 150 ℃.
3. Phosphorus mud enters a screw conveyor through a discharge hole of a storage tank, the phosphorus mud is conveyed to a primary hollow blade dryer when the screw conveyor rotates, the phosphorus mud slowly enters a secondary hollow blade dryer along with the rotation of the dryer, and the temperature in the secondary hollow blade dryer reaches 300 ℃; the phosphorus mud is gradually heated, and finally, the elemental phosphorus in the phosphorus mud is evaporated, and the residue is discharged from a slag outlet of the secondary hollow blade dryer.
4. And (4) introducing gas from the upper parts of the primary and secondary hollow blade dryers into a spray absorption tower for cooling and absorption to obtain the yellow phosphorus.
5. The heat conducting oil is used for heating the secondary hollow blade drying machine in the whole process, the primary temperature is controlled at the room temperature of 110-350 ℃, and the secondary temperature is controlled at the temperature of 280-350 ℃.
Example 1
Starting the yellow phosphorus tail gas organic heat carrier furnace, heating the heat transfer oil to 320 ℃, adjusting the rotating speed of the dryer to 4r/min, adjusting the temperature in the first-stage hollow blade dryer to 150 ℃, and starting the screw pump to carry the phosphorus mud (P) to the dryer in a speed of 0.8m per hour205The content is 3.2). After 8 hours of heating, residues come out from a slag outlet of the secondary hollow blade dryer, the total phosphorus content (counted by P) in the residues is 6.6 percent, the residues are placed in the air without smoking, and the purity of yellow phosphorus is 99.95 percent.
Example 2
Starting the yellow phosphorus tail gas organic heat carrier furnace, heating the heat transfer oil to 320 ℃, adjusting the rotating speed of the dryer to 5r/min, enabling the temperature in the first-stage hollow blade dryer to reach 150 ℃, and starting the screw pump to carry the phosphorus mud (P) to the dryer in a speed of 0.8m per hour205The content was 2.8). After heating for 7 hours and 20 minutes, residues come out from a slag outlet of the secondary hollow blade dryer, the total phosphorus content (counted by P) in the residues is 6.3 percent, the residues are placed in the air without smoking, and the purity of yellow phosphorus is 99.94 percent.
Example 3
Starting the yellow phosphorus tail gas organic heat carrier furnace, heating the heat transfer oil to 320 ℃, adjusting the rotating speed of the dryer to 6r/min, enabling the temperature in the first-stage hollow blade dryer to reach 150 ℃, and starting the screw pump to carry the phosphorus mud (P) to the dryer in a speed of 0.8m per hour205The content was 3.0). After 6 hours and 40 minutes of heating, residues come out from a slag outlet of the secondary hollow blade dryer, the total phosphorus content (counted by P) in the residues is 6.7 percent, the residues are placed in the air without smoking, and the purity of yellow phosphorus is 99.95 percent.

Claims (8)

1. The process is characterized in that the device used in the process is structurally characterized in that a phosphorus mud inlet pipeline is connected with a screw stacking machine (1), the screw stacking machine (1) is connected with a first blade dryer (3) through a first screw feeder (2), and the first blade dryer (3) is connected with a second blade dryer (4);
the heat conduction oil pipeline and the heat medium storage tank (6) are connected with a gas boiler (8) through a hot oil pump (7), the gas boiler (8) is respectively connected with the bottoms of the first blade dryer (3) and the second blade dryer (4), and the tops of the first blade dryer (3) and the second blade dryer (4) are respectively converged with a pipeline from the gas boiler (8) through pipelines and then are connected with the heat medium storage tank (6);
the method comprises the following steps of evaporating element phosphorus from phosphorus mud by utilizing an evaporation principle so as to achieve the purpose of recycling yellow phosphorus, dehydrating the phosphorus mud by a dehydration device, transferring the phosphorus mud into a phosphorus mud storage tank, enabling the phosphorus mud to enter a primary paddle dryer from a discharge port of the storage tank by a screw feeder to evaporate water, enabling the phosphorus mud to automatically flow into a secondary paddle dryer through a slag outlet of the primary paddle dryer to evaporate the element phosphorus, enabling a star-shaped feeder to discharge slag from the slag outlet of the secondary paddle dryer, and directly burying the evaporated residue or processing the evaporated residue into a compound fertilizer by a fertilizer factory; the heating medium is heated by the heating device, flows into the primary paddle dryer through the centrifugal pump and the secondary paddle dryer, and returns to the heating medium storage tank for recycling; and the evaporated gas of the primary blade dryer and the secondary blade dryer enters a washing tower tank to be condensed to recover water vapor and yellow phosphorus, the drying temperature of the phosphorus mud passing through the primary blade dryer is 110-350 ℃, and the drying temperature of the secondary blade dryer is 280-350 ℃.
2. The process of the device for the continuous multi-stage evaporation recovery of yellow phosphorus in phosphorus mud according to claim 1, wherein the tops of the first paddle dryer (3) and the second paddle dryer (4) are respectively connected with the washing tower tank (10) through pipelines, the gas inlet pipeline outside the battery compartment is connected with a gas boiler (8), and the gas boiler (8) is connected with a chimney (9); an external clean water pipeline is connected with the upper part of the washing tower groove (10), an external steam pipeline is connected with the lower part of the washing tower groove (10), and the top of the washing tower groove (10) is connected with the chimney (9); the upper part of the washing tower groove (10) is connected with a yellow phosphorus sewage pool outside the overflow boundary area, and the lower part is connected with a condensed water discharge pipe.
3. A process carried out by the device for continuously recovering yellow phosphorus from phosphorus sludge by multistage evaporation as claimed in claim 1, wherein nitrogen gas inlet pipes are arranged at the tops of the screw feeder (2), the first paddle dryer (3) and the second paddle dryer (4).
4. A process carried out by the device for continuously evaporating and recovering yellow phosphorus in phosphorus mud in multiple stages as claimed in claim 1, wherein the bottom of the second blade dryer (4) is connected to the waste residue bin through the second screw feeder (11).
5. A process carried out by an apparatus for the continuous multi-stage evaporation recovery of yellow phosphorus from phosphorus sludge as claimed in claim 1, wherein the screw stacking machine (1) is connected to a yellow phosphorus wastewater tank outside the overflow boundary zone.
6. The process performed by the device for recovering yellow phosphorus from phosphorus mud by continuous multistage evaporation according to claim 1, wherein the paddle dryer is hollow, the heat medium fluid is used for indirectly heating the phosphorus mud, the three-stage sealing is respectively used for sealing two ends of the paddle by using the filler, the inert gas and the filler, so that the air is prevented from contacting with the phosphorus mud, the heat medium fluid two-stage hollow paddle dryer flows into the one-stage hollow paddle dryer, and the two-stage heat source is used in series.
7. The process of claim 1, wherein the phosphorus sludge stays in the primary hollow blade dryer for 2-4 hours and in the secondary hollow blade dryer for 3-8 hours.
8. The process carried out by the device for continuously evaporating and recovering the yellow phosphorus in the phosphorus mud in multiple stages as claimed in claim 1, wherein the heat transfer fluid is heat transfer oil and steam.
CN201710995305.4A 2017-10-23 2017-10-23 Device and method for continuously recovering yellow phosphorus in phosphorus mud through multistage evaporation Active CN107601446B (en)

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CN112506158A (en) * 2020-12-14 2021-03-16 云南煜锜环保科技有限公司 Automatic mud phosphorus distillation temperature control system

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CN103043638A (en) * 2013-01-06 2013-04-17 中石化南京工程有限公司 Novel continuous phosphorus filtration technology with filter pressing method and production device of technology
CN203128203U (en) * 2013-01-16 2013-08-14 湖北兴发化工集团股份有限公司 Device for extracting yellow phosphorus via reduced pressure distillation of phosphorus sludge
CN203683095U (en) * 2014-01-28 2014-07-02 湖北兴发化工集团股份有限公司 Equipment for continuously evaporating and recovering yellow phosphorus in phosphorus sludge
CN105984860A (en) * 2015-02-06 2016-10-05 云南天安化工有限公司 Method for recovering and refining yellow phosphorus by phosphorus sludge
CN105883736A (en) * 2016-04-11 2016-08-24 云南澄江磷化工广龙磷酸盐厂 Efficient and low-pollution phosphorous-slurry recycling method
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