CN115108540B - Method and formula for improving separation efficiency and quality of sludge phosphorus at low temperature - Google Patents
Method and formula for improving separation efficiency and quality of sludge phosphorus at low temperature Download PDFInfo
- Publication number
- CN115108540B CN115108540B CN202210696302.1A CN202210696302A CN115108540B CN 115108540 B CN115108540 B CN 115108540B CN 202210696302 A CN202210696302 A CN 202210696302A CN 115108540 B CN115108540 B CN 115108540B
- Authority
- CN
- China
- Prior art keywords
- phosphorus
- extractant
- liquid
- particles
- valve
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for improving the separation efficiency and quality of phosphorus mud at low temperature, which adopts a double extraction process to treat phosphorus mud respectively, wherein an extractant I in a first extraction process is used for destroying a colloidal film protective layer coated on the surface of phosphorus particles or other solid particles, so that the phosphorus particles or other solid particles coated by the colloidal film protective layer are exposed in phosphorus mud liquid, and the phosphorus particles and other solid particles are precipitated at the lower part of the phosphorus mud liquid by dead weight and separated from the colloidal film protective layer; the extractant II in the second extraction process is used for dissolving the phosphorus particles in the extractant II to form suspension liquid, and then the centrifugation operation is carried out to realize the purpose of separation in a low-temperature state.
Description
Technical Field
The invention relates to the technical field of solid-liquid separation of sludge phosphorus, in particular to a method and a formula for improving the separation efficiency and quality of sludge phosphorus at low temperature.
Background
The sludge phosphorus is one of main byproducts generated in the yellow phosphorus production process, belongs to dangerous solid waste in phosphorus chemical industry, and is an important problem in the yellow phosphorus production, which not only affects the recovery rate and the production cost of phosphorus in the yellow phosphorus industrial production, but also causes serious environmental pollution problem, so almost all domestic yellow phosphorus manufacturers are discussing the treatment and the utilization of the sludge phosphorus so as to achieve good environmental benefit, economic benefit and social benefit, thereby realizing the strategy metagraph of sustainable development of human beings.
The company applied for a patent (application number: 2021110915702) for a low-temperature solid-liquid separation method and a medicament formula for phosphorus mud in 2021, 9 months, and the following defects are found in the actual application of the technology in two years:
firstly, injecting an extractant (carbon disulfide) into a dissolving tank, mixing the extractant with the phosphorus mud, starting a stirrer to uniformly mix the mixed solution, and standing for 100-150min to fully mix the extractant with the phosphorus mud; the standing time is too long, and the extractant and the phosphorus are not fully mixed;
secondly, the required amount of the extractant (carbon disulfide) is particularly large, the industrial cost is increased, the centrifugation process period is long due to the use of a large amount of the extractant (carbon disulfide), and the equipment maintenance rate is high;
thirdly, the yellow phosphorus obtained after separation is low in quality.
Disclosure of Invention
The invention aims to provide a method and a formula for improving the separation efficiency and quality of sludge phosphorus at low temperature, so as to overcome the defects of the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the method adopts double extraction processes to treat phosphorus mud respectively, wherein an extractant I in a first extraction process is used for destroying a colloidal film protective layer coated on the surface of phosphorus particles or other solid particles, so that the phosphorus particles or other solid particles coated by the colloidal film protective layer are exposed in phosphorus mud liquid, and the phosphorus particles and other solid particles are precipitated at the lower part of the phosphorus mud liquid by dead weight and separated from the colloidal film protective layer; the extractant II in the second extraction process is used for dissolving the phosphorus particles in the extractant II to form suspension liquid, and then the centrifugation operation is carried out to realize the purpose of separation in a low-temperature state.
As a further aspect of the invention: the first extractant and the second extractant are mutually incompatible.
As a further aspect of the invention: the first extractant adopts coconut oil fatty acid diethanolamide.
As a further aspect of the invention: the extractant II adopts carbon disulfide.
As a further aspect of the invention: the separation method comprises the steps of preliminary preparation, dissolution, low-temperature solid-liquid separation, rectification, and final product refining, rinsing, storage and packaging.
As a further aspect of the invention: the neutral sodium chloride solution is added in the preparation process in the earlier stage, and the time of the extraction process can be shortened and the production period can be shortened by adding the sodium chloride solution.
As a further aspect of the invention: the preparation process in the early stage is to add an extractant into a storage tank to mix and perform a first extraction process after the sludge phosphorus in the storage tank is heated and dissolved by hot water or steam, so that organic matters suspended in the sludge phosphorus liquid and organic matters coated in a colloidal film protection layer on the surface of phosphorus particles or other solid particles are dissolved in the extractant I, organic matters in the phosphorus sludge liquid are separated from the phosphorus particles and other solid particles, then a dissolving process is performed, namely the sludge phosphorus liquid is sent to a dissolving tank by a submerged pump, the materials pumped into the dissolving tank are kept stand for 25-40min by utilizing the characteristic of material specific gravity difference, all phosphorus is settled at the bottom of the dissolving tank, water is positioned at the upper part, the sludge phosphorus is isolated from air, the occurrence of yellow phosphorus spontaneous combustion phenomenon is avoided, a cold sewage circulating pump is started to operate, the cold sewage pump is sent to a dissolving tank to replace hot water for cooling, the replaced hot water overflows from an overflow port of the top of the dissolving tank until the temperature of the dissolving tank is reduced to 20-28 ℃.
As a further aspect of the invention: the low-temperature solid-liquid separation procedure carries out a second extraction process by mixing the extractant II with the phosphorus mud, the suspension liquid formed after mixing is put into a centrifuge, whether the filter cloth of the centrifuge is flat or not is checked before feeding, and then a centrifuge cover is covered; the nitrogen valve is opened, nitrogen replacement is carried out on the inside of the cavity of the centrifugal machine and the rear end of the material conveying pipe valve until the oxygen content is less than or equal to 0.2%, the water spraying valve is opened, flowing water flows in along the inner wall, and a spray header arranged in the cavity of the centrifugal machine after the valve is opened enables the cavity of the centrifugal machine to be in atomized spraying; in order to avoid static electricity generated by friction, the static electricity is grounded, after the centrifugal machine is started to run normally in no-load, a manual valve of a discharging valve of the dissolving tank is opened, when the oxygen content is less than or equal to 0.2%, an automatic valve is automatically opened in a linkage manner, materials automatically flow into a cavity of the centrifugal machine from a conveying pipe of the dissolving tank for centrifugal separation, filtrate automatically flows into a heater through a U-shaped liquid seal device, and a filter screen is cleaned through clear water.
The core principle of the technical scheme is as follows: firstly, hot water or steam heating and dissolving are carried out on phosphorus mud, so that effective substances such as phosphorus particles and the like can be fully dispersed and suspended in liquid, and coconut fatty acid diethanolamide (extractant I) is added and stirred in a first extraction process, so that the method has four obvious effects: firstly, organic matter parts in a colloidal film protection layer coated on the surfaces of phosphorus particles or other solid particles can be fused and destroyed by an extractant, so that the phosphorus particles or other solid particles can be completely exposed in liquid, and the recovery of the phosphorus particles is realized; secondly, the extractant I can absorb organic matters in the colloidal film protection layer coated on the surfaces of the phosphorus particles or other solid particles and can also absorb other organic matters in the liquid, so that the extractant II can conveniently extract the phosphorus particles rapidly due to no (or less) organic matters in the second extraction process; thirdly, in the first extraction process, phosphorus particles or other solid particles can be completely exposed in liquid under the action of the first extractant, at the moment, the phosphorus particles can be fused into the liquid in a suspension state, the solid particles with higher specific gravity sink to the lower part, the solid particles with lower specific gravity float to the upper part, and the liquid with higher content of the phosphorus particles is extracted for subsequent processes, so that the reaction time of the extractant II (carbon disulfide) is greatly shortened, and meanwhile, the extracted substances contain less other solid particles, so that the recovery quality of phosphorus is greatly improved; fourthly, the extractant can achieve thickening and can increase water solubility and stability.
Compared with the prior art, the invention has the beneficial effects that: the invention uses the physical property of materials in the whole process of recycling the products, has no chemical reaction and other products in the process, basically realizes full-sealing operation in operation, has no pollution on site, is the most ideal process for solving the phosphorus mud treatment process in the yellow phosphorus industry, has great potential and great profitability for leading the market after the technological breakthrough.
Drawings
FIG. 1 is a schematic view of a dissolution process flow of the present invention;
FIG. 2 is a schematic diagram of a low temperature solid-liquid process flow in accordance with the present invention;
fig. 3 is a schematic block diagram of the process flow of the rectification process of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a technical scheme that:
the method utilizes the property that yellow phosphorus is easy to dissolve in carbon disulfide (solvent) and the property that organic matters are easy to dissolve in coconut fatty acid diethanolamide, is operated through the processes of dissolving, filtering, distilling and the like in the experimental process, obtains ideal data through numerous tests, runs through a pilot plant (the using equipment is a pilot plant expansion test such as an enamel stirring kettle, a centrifuge, a reboiler, a condenser, a recoverer and the like at the moment), and has very smooth progress, the recovery rate of the solvent is more than 95%, the quality purity content of the product is 99.8% (the qualified product is 99.95%), and the product can reach the qualified product after being treated through a refining process.
At present, the technology has more patents on the net, but industrialized production devices are not yet developed, in recent years, the national regulations on the discharge behavior of environmental protection pollutants are strict, the coming-out policy is aggravated year by year, the advanced process for treating the byproduct phosphorus mud in the yellow phosphorus industry is urgent, however, the method uses the physical property of materials in the whole process of processing and recycling products, the process has no chemical reaction and other products, the full-sealing operation is basically realized in operation, the field has no pollution, the technology is the most ideal technology for solving the phosphorus mud treatment technology in the yellow phosphorus industry, and after the technological breakthrough, the market supply and the shortage have great potential and great profitability for leading the market.
According to the low-temperature solid-liquid separation method for the sludge phosphorus, which is disclosed in the embodiment, the physical characteristics of R=10, boiling point and large density difference of yellow phosphorus in carbon disulfide are utilized, solid-phase yellow phosphorus in the sludge phosphorus is rapidly dissolved under the low-temperature condition, yellow phosphorus in the sludge phosphorus is dissolved into a liquid phase and deposited at the bottom of a container, solid-phase dust is suspended in a liquid seal middle layer, after standing and layering, phosphorus-containing solution is conveyed to a rectification procedure for rectification through centrifugal separation equipment, carbon disulfide with a lower boiling point continuously overflows from the top of the tower through heating, and enters a condensation recovery system for recycling;
in the rectification process, as the boiling point of the carbon disulfide is lower, the carbon disulfide rapidly escapes from the liquid level, the R value is continuously reduced, yellow phosphorus is continuously separated out along with the change of the R reduction, and finally, after the rectification of the carbon disulfide is finished, the rest materials of the rectification equipment are yellow phosphorus and water, and the yellow phosphorus is further refined and rinsed through the conveying equipment until the materials are qualified.
The production process comprises the following steps:
4. operation indexes:
the main production device of the device comprises a dissolving process, a low-temperature solid-liquid separation process, a rectifying process, and the refining, rinsing, storage and packaging of the final product.
The following process flow is described according to the procedures:
1. early preparation step
The mud phosphorus in the storage tank is heated and dissolved by hot water or steam, then the coconut oil fatty acid diethanolamide is added and stirred for the first extraction process, so that organic matters suspended in the mud phosphorus liquid and organic matters coated in a colloidal film protection layer on the surface of phosphorus particles or other solid particles are dissolved in the coconut oil fatty acid diethanolamide, and the separation of organic matters in the phosphorus mud liquid from the phosphorus particles and other solid particles is realized; other solid particles are layered by their own weight, while the phosphorus particles are suspended in the liquid
1. Process flow block diagram of dissolution procedure
1. The process flow diagram of the dissolution process is shown in fig. 1 below:
2. overview of the dissolution procedure
First, 1m of cold sewage and 1m3 of sodium chloride solution (20%) were injected into a dissolution tank (stirred tank). After the sludge phosphorus in the storage tank is heated and dissolved by hot water or steam, the sludge phosphorus is pumped into a dissolving tank (existing) by a submerged pump, the materials pumped into the dissolving tank are kept stand for 30min by utilizing the characteristic of the difference of specific gravity of the materials, the sludge phosphorus is settled at the bottom of the dissolving tank due to the high specific gravity (1.5 g/m < 3 >) after standing, the water is positioned at the upper part, the sludge phosphorus is isolated from air, the spontaneous combustion phenomenon of yellow phosphorus is avoided, a cold sewage circulating pump is started to operate, cold sewage is pumped into the dissolving tank to replace hot water for cooling, the replaced hot water overflows to a cold sewage tank from a top overflow port, and the temperature of the dissolving tank is reduced until the temperature of the dissolving tank is reduced to 25 ℃.
When the temperature of the dissolving tank is reduced to 25 ℃, a valve from a nitrogen making machine is opened, air replacement is carried out on the dissolving tank until the oxygen content is less than or equal to 0.2%, then a bottom valve of an extractant collector is slowly opened, the extractant metered by a liquid level sensor is mixed with the phosphorus mud in the dissolving tank according to the proportion of 100:11, a stirrer is started to uniformly mix the mixed solution, and the mixture is kept stand for 120min, so that the solvent is fully mixed with the phosphorus mud.
2. Process flow block diagram of low-temperature solid-liquid separation procedure
1. Process flow block diagram of low temperature solid-liquid separation process 2:
2. overview of the technological process of the low-temperature solid-liquid separation procedure
Before feeding, opening the centrifuge, checking whether the filter cloth of the centrifuge is flat, and then covering the centrifuge with a cover. The method comprises the steps of opening a nitrogen valve, carrying out nitrogen replacement on the inside of a centrifugal machine cavity and the rear end of a material conveying pipe valve until the oxygen content is less than or equal to 0.2%, opening a water spraying valve (flowing in along the inner wall), enabling a spray header arranged in the centrifugal machine cavity to be in atomized spraying (static electricity is generated by friction and grounded) after the valve is opened, inputting the frequency of the centrifugal machine to 25hz, starting the centrifugal machine to perform idle normal operation, opening a manual valve of a discharging valve of a dissolving tank, automatically opening a chain automatic valve when the oxygen content is less than or equal to 0.2%, enabling materials to automatically flow from the material conveying pipe of the dissolving tank into the centrifugal machine cavity for centrifugal separation, enabling filtrate to automatically flow into a heater through a U-shaped liquid seal, and cleaning the filter screen through clear water
Before the second feeding, an automatic emptying valve of an inlet pipe of the centrifugal machine is opened, nitrogen is slightly filled into the cavity of the centrifugal machine for replacement until the oxygen content is less than or equal to 0.2%, water is filled into the cavity of the centrifugal machine, the centrifugal machine is opened, whether filter cloth of the centrifugal machine is leveled or replaced is checked, and then a cover of the centrifugal machine is covered. The method comprises the steps of opening a nitrogen valve, carrying out nitrogen replacement on the inside of a centrifugal machine cavity and the rear end of a material conveying pipe valve until the oxygen content is less than or equal to 0.2%, opening a water spraying valve, enabling a spray header arranged in the centrifugal machine cavity to enable the inside of the centrifugal machine cavity to be in atomized spraying after the valve is opened, inputting the frequency of the centrifugal machine to be 25hz, starting a manual valve of a discharging valve of a dissolving tank after the centrifugal machine runs normally empty, and automatically opening a chain automatic valve when the oxygen content is less than or equal to 0.2%, wherein materials automatically flow from the material conveying pipe of the dissolving tank to the inside of the centrifugal machine cavity for centrifugal separation, and filtrate automatically flows into a heater through a U-shaped liquid seal device.
3. Schematic diagram of process flow block of rectification procedure
1. Schematic diagram 3 of process flow block of rectification procedure
2. Technical flow outline of rectification procedure:
the heater is prepared before the centrifuge is started. Firstly, injecting clean water (buffer, static elimination) of 30-40cm into a heater (water injection pipe), and then replacing the inside of the heater by nitrogen from a nitrogen making machine; until the oxygen content is replaced to be less than or equal to 0.2 percent (synchronous replacement with the centrifugal machine), at the moment, materials from the centrifugal machine automatically flow into the heater by utilizing the high level difference, after the materials flow out, the centrifugal machine is stopped, the self-regulating valve of the outlet of the centrifugal machine is remotely closed, the water inlet self-regulating valve of the centrifugal machine is opened through remote control, the centrifugal machine is immediately filled with water, and the situation that the residual medicament in the centrifugal machine is volatilized continuously to cause mixed gas explosion injury is generated when the centrifugal machine cover is uncovered when the filter cake of the centrifugal machine is cleaned is ensured.
After the water in the cavity of the centrifugal machine is filled, a nitrogen valve from a nitrogen making machine is slowly opened, nitrogen is slightly filled into the heater, a steam valve from a boiler is opened, steam heats materials in the heater through a steam coil pipe, extractant in the materials continuously volatilizes and escapes from the water surface due to the temperature rise, the extractant enters a condenser, and after the gasified and volatilized extractant enters the condenser, the extractant continuously liquefies to form a liquid state, and the liquefied extractant automatically flows to a recovery tank filled with water for storage and recycling. The system pressure is emptied through the breather valve at the top of the recovery tank, after the extraction agent is completely volatilized, the distilled residues in the heater are yellow phosphorus and water, the products are remotely controlled through the remote control valve, the valve at the bottom of the heater is opened, the products automatically flow into the liquid seal tank, and then the products are refined through pumping to a refining process, and the refined qualified products are packaged and sold.
The rectification procedure starts the following operation after the steam is more than or equal to 0.3 Mpa:
1. opening the inlet and outlet valves of the cooler, starting the cooling water pump and enabling the cooling water to circulate normally;
2. slightly opening a nitrogen valve and replacing the inside of the heater; in the rectification process, the nitrogen valve is kept slightly normally open, and the internal pressure of the heater is positive.
3. And (3) opening a drain valve of the steam outlet and discharging condensed water in the pipe, and closing the drain valve after the condensed water is discharged. Then the inlet valve is slowly opened, and steam is introduced into the heater. Closing a steam inlet valve when the temperature in the heater reaches 30 ℃, and keeping the temperature constant for 40min; observing and recording the recovery amount of the extractant; then slowly opening the steam inlet valve, closing the steam inlet valve after the temperature of the heater reaches 50 ℃, and keeping the temperature for 40 minutes; observing and recording the recovery amount of the extractant; slowly opening the steam inlet valve again, slowly heating to 80 ℃, closing the steam inlet valve, and keeping the temperature for 30min; observing and recording the recovery amount of the extractant; calculating the ratio of the dissolved addition amount to the recovery amount, sampling the mixture through a heater outlet sampling valve after the ratio reaches 70-80%, rinsing the mixture with cooling water, and observing the cooling condition of the separated phosphorus.
4. In the rectification process of the heater, the temperature in the heater is well controlled, the overhigh temperature is avoided in the initial stage, and the recovery of the solvent is not facilitated.
5. The temperature of the condenser in the rectification process is the normal temperature of water (the lower the temperature is, the better the temperature is, the refrigerant can be selected according to the situation), and the pressure is 120-130kpa.
3. The system automatically controls the linkage requirement:
1. the pressure of the dissolving tank is more than or equal to 0.1MPa, and the dissolving tank emptying valve is opened and interlocked;
2. the oxygen content in the centrifuge is less than or equal to 0.2 percent and is linked with a feed valve;
3. the temperature of the heater is interlocked with the steam inlet self-regulating valve;
4. description of the device composition
1. Dissolving tank)
1. A site thermometer, a pressure gauge, a liquid level gauge, a remote temperature, a remote pressure, a remote liquid level gauge and an oxygen content analyzer;
2. the automatic emptying valve and the fire arrestor on the automatic emptying valve are intermittently emptying, and no open fire exists in the range of more than 3m or 10 m above the platform;
3. a solvent adding pipe and valve, a phosphorus injecting pipe and valve, a cleaning water pipe and valve;
4. dissolution tank outlet: a manual valve, an automatic shut-off valve, a sight glass valve and a cleaning water pipe joint;
2. centrifuge with a separator
1、≤0.2％；
2. The electrostatic resistance is less than or equal to 1 omega.
3. A) a heater
1. A site thermometer, a pressure gauge, a liquid level gauge, a remote transmission temperature display, a remote transmission pressure display, a remote transmission liquid level display and a remote transmission oxygen content analyzer;
2. heater outlet tube: two manual valves, a blow-down valve and a sight glass valve.
The construction and operation process of the production device comprises the following steps:
after pilot test is finished, the team rapidly adjusts the industrial structure through acute market insight, on the basis of ensuring that the building and security industry has a growth rate, the industries such as chemical industry, environmental protection and the like rapidly enter the arming industry, a set of production device is built in the next year, but due to weak technical strength of the team profession and insufficient knowledge of production equipment and technology, several safety and temporary accidents occur in sequence in the production process, and the reasons of the accidents are summarized as follows:
1. the nitrogen content of the purchased nitrogen making unit is only 86% through chromatographic analysis comparison, and therefore, two explosions occur in the centrifugal separation process.
2. The dissolution tank is processed and installed by self, due to unreasonable arrangement and illegal operation of operators, in the process of rechecking, under the condition that nitrogen is not added and water is not sealed in the dissolution tank, the operators uncover the water seal cover of the dissolution tank, so that the concentrated solvent gas volatilized in the tank overflows the tank body, and flash explosion occurs.
The debugging work exposes various reasons of unreasonable equipment selection, unsafe equipment design, insufficient understanding of solvent properties and harmfulness by operators and the like, so that the debugging is stopped, a person with knowledge about the operation of the carbon disulfide industry and experience in equipment needs to be searched for to be added into a team for management and operation, and collusion development is carried out.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for improving the separation efficiency and quality of sludge phosphorus at low temperature is characterized by comprising the following steps: the method adopts a double extraction process to treat phosphorus mud respectively, wherein an extractant I in a first extraction process is used for destroying a colloidal film protective layer coated on the surfaces of phosphorus particles or other solid particles, so that the phosphorus particles or other solid particles coated by the colloidal film protective layer are exposed in phosphorus mud liquid, and the phosphorus particles and other solid particles are precipitated at the lower part of the phosphorus mud liquid by dead weight and are separated from the colloidal film protective layer; the extractant II in the second extraction process is used for dissolving the phosphorus particles in the extractant II to form suspension liquid, and then the centrifugation operation is carried out to realize the separation purpose in a low-temperature state; the extractant I is coconut oil fatty acid diethanolamide, and the extractant II adopts carbon disulfide.
2. The method for improving the separation efficiency and quality of the sludge phosphorus at low temperature according to claim 1, which is characterized in that: the extractant I and the extractant II are mutually insoluble.
3. A method for improving the separation efficiency and quality of sludge phosphorus at low temperature according to any one of claims 1-2, characterized in that: the separation method comprises the steps of preliminary preparation, dissolution, low-temperature solid-liquid separation, rectification, and final product refining, rinsing, storage and packaging.
4. A method for improving the separation efficiency and quality of sludge phosphorus at low temperature according to claim 3, wherein: the preparation process in the early stage is to add an extractant into a storage tank to mix and perform a first extraction process after the sludge phosphorus in the storage tank is heated and dissolved by hot water or steam, so that organic matters suspended in the sludge phosphorus liquid and organic matters coated in a colloidal film protection layer on the surface of phosphorus particles or other solid particles are dissolved in the extractant I, organic matters in the phosphorus sludge liquid are separated from the phosphorus particles and other solid particles, then a dissolving process is performed, namely the sludge phosphorus liquid is sent to a dissolving tank by a submerged pump, the materials pumped into the dissolving tank are kept stand for 25-40min by utilizing the characteristic of material specific gravity difference, all phosphorus is settled at the bottom of the dissolving tank, water is positioned at the upper part, the sludge phosphorus is isolated from air, the occurrence of yellow phosphorus spontaneous combustion phenomenon is avoided, a cold sewage circulating pump is started to operate, the cold sewage pump is sent to a dissolving tank to replace hot water for cooling, the replaced hot water overflows from an overflow port of the top of the dissolving tank until the temperature of the dissolving tank is reduced to 20-28 ℃.
5. A method for improving the separation efficiency and quality of sludge phosphorus at low temperature according to claim 3, wherein: the low-temperature solid-liquid separation procedure carries out a second extraction process by mixing the extractant II with the phosphorus mud, the suspension liquid formed after mixing is put into a centrifuge, whether the filter cloth of the centrifuge is flat or not is checked before feeding, and then a centrifuge cover is covered; the nitrogen valve is opened, nitrogen replacement is carried out on the inside of the cavity of the centrifugal machine and the rear end of the material conveying pipe valve until the oxygen content is less than or equal to 0.2%, the water spraying valve is opened, flowing water flows in along the inner wall, and a spray header arranged in the cavity of the centrifugal machine after the valve is opened enables the cavity of the centrifugal machine to be in atomized spraying; in order to avoid static electricity generated by friction, the static electricity is grounded, after the centrifugal machine is started to run normally in no-load, a manual valve of a discharging valve of the dissolving tank is opened, when the oxygen content is less than or equal to 0.2%, an automatic valve is automatically opened in a linkage manner, materials automatically flow into a cavity of the centrifugal machine from a conveying pipe of the dissolving tank for centrifugal separation, filtrate automatically flows into a heater through a U-shaped liquid seal device, and a filter screen is cleaned through clear water.
6. A method for improving the separation efficiency and quality of sludge phosphorus at low temperature according to claim 3, wherein: neutral sodium chloride solution is added in the preparation process.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111091570.2A CN113816348A (en) | 2021-09-17 | 2021-09-17 | Low-temperature solid-liquid separation method for phosphorus sludge and medicament formula |
| CN2021110915702 | 2021-09-17 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115108540A CN115108540A (en) | 2022-09-27 |
| CN115108540B true CN115108540B (en) | 2023-05-30 |
Family
ID=78922325
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111091570.2A Pending CN113816348A (en) | 2021-09-17 | 2021-09-17 | Low-temperature solid-liquid separation method for phosphorus sludge and medicament formula |
| CN202210696302.1A Active CN115108540B (en) | 2021-09-17 | 2022-06-17 | Method and formula for improving separation efficiency and quality of sludge phosphorus at low temperature |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111091570.2A Pending CN113816348A (en) | 2021-09-17 | 2021-09-17 | Low-temperature solid-liquid separation method for phosphorus sludge and medicament formula |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN113816348A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071394A (en) * | 1992-09-30 | 1993-04-28 | 李兴德 | From phosphorus mud, reclaim the method for yellow phosphorus |
| CN1428294A (en) * | 2002-11-04 | 2003-07-09 | 杨烨 | Chemical method for extracting yellow phosphorus from phosphorus mud |
| CN103588185A (en) * | 2013-11-14 | 2014-02-19 | 云南江磷集团股份有限公司 | Method for removing sulfur from yellow phosphorus |
| CN104555956A (en) * | 2014-12-25 | 2015-04-29 | 湖北兴发化工集团股份有限公司 | Method and equipment for recycling yellow phosphorus from phosphorus mud |
-
2021
- 2021-09-17 CN CN202111091570.2A patent/CN113816348A/en active Pending
-
2022
- 2022-06-17 CN CN202210696302.1A patent/CN115108540B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071394A (en) * | 1992-09-30 | 1993-04-28 | 李兴德 | From phosphorus mud, reclaim the method for yellow phosphorus |
| CN1428294A (en) * | 2002-11-04 | 2003-07-09 | 杨烨 | Chemical method for extracting yellow phosphorus from phosphorus mud |
| CN103588185A (en) * | 2013-11-14 | 2014-02-19 | 云南江磷集团股份有限公司 | Method for removing sulfur from yellow phosphorus |
| CN104555956A (en) * | 2014-12-25 | 2015-04-29 | 湖北兴发化工集团股份有限公司 | Method and equipment for recycling yellow phosphorus from phosphorus mud |
Non-Patent Citations (2)
| Title |
|---|
| 底泥磷释放的影响因素;姜敬龙;吴云海;;环境科学与管理(06);全文 * |
| 瘠性磷矿渣生产气泡混合轻质土的试验研究;李明东;范公俊;姬凤玲;田安国;;重庆交通大学学报(自然科学版)(05);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115108540A (en) | 2022-09-27 |
| CN113816348A (en) | 2021-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105237401B (en) | A kind of manufacture craft of plasticizer | |
| CN106281396B (en) | Waste plastic cracking equipment and method | |
| CN104453747A (en) | Resource utilization method of oil and gas field well drilling abandoned oil-base mud | |
| CN106693618B (en) | The harmless processing system of process tail gas and exhaust gas during a kind of coal tar deep processing | |
| CN102504851B (en) | Equipment and process for producing light tar by controlling QI (Quality Index) value of tar | |
| CN107651817A (en) | Oil-containing dross sludge treating system and technique | |
| CN209602346U (en) | A kind of oil sludge and sand minimizing processing unit | |
| CN115108540B (en) | Method and formula for improving separation efficiency and quality of sludge phosphorus at low temperature | |
| CN205974397U (en) | Oily waste water carclazyte sediment treatment facility | |
| CN208449017U (en) | A kind of VOC recycling reprocessing device | |
| CN106915891A (en) | A kind of oil plant oily sludge is innoxious and processing method of resource | |
| CN101811745A (en) | Treating device for extracting naphthalene sulfonic acid waste liquor | |
| CN104891756B (en) | Based on the Fatlute recovering device and method being sufficiently stirred for | |
| CN103285734B (en) | A treatment process and a system for waste organic solvents based on nano filter membranes | |
| CN205953929U (en) | Waste mineral oil treatment facility | |
| CN205893165U (en) | Microwave radiation rubbish pyrolysis treatment device | |
| CN208748026U (en) | A kind of petroleum vapor recovery lime set is collected and conveying device | |
| CN208886800U (en) | A kind of trash burning processing unit in furfural production line | |
| RU125882U1 (en) | INSTALLATION FOR ADDITION OF ADDITIVES IN OIL PIPELINE | |
| CN207713610U (en) | A kind of sludge reduction processing system | |
| CN107935817B (en) | Device and method for recovering isooctyl alcohol from isooctyl p-dimethylaminobenzoate crude product | |
| CN109201023A (en) | Sewage filtering material regenerating unit | |
| CN205528619U (en) | Oil plant effluent oil treatment system | |
| CN113020228A (en) | Benzene tank bottom residue treatment system and treatment process | |
| CN216726620U (en) | Tail gas treatment system of asphalt mixture plant-mixing heat regeneration equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20221209 Address after: Room 402, Unit 5, Building 3, Sunshine Garden, No. 12, Huancheng South Road, Chengguan Town, Kaiyang County, Guiyang City, Guizhou Province 550300 Applicant after: Wang Ronghua Address before: 550000 No. 2, floor 4, unit 5, building 3, Shengli Xiguang Garden community, Zijiang neighborhood committee, Yunkai street, Kaiyang County, Guiyang City, Guizhou Province Applicant before: Guizhou trenqing Technology Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230330 Address after: 550300 No. 2, Floor 4, Unit 5, Building 3, Shengli Xiguang Garden Community, Zijiang Neighborhood Committee, Yunkai Street, Kaiyang County, Guiyang City, Guizhou Province Applicant after: Guizhou trenqing Technology Co.,Ltd. Address before: Room 402, Unit 5, Building 3, Sunshine Garden, No. 12, Huancheng South Road, Chengguan Town, Kaiyang County, Guiyang City, Guizhou Province 550300 Applicant before: Wang Ronghua |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |