CN211644817U - Yellow phosphorus wastewater treatment and cyclic utilization's device - Google Patents
Yellow phosphorus wastewater treatment and cyclic utilization's device Download PDFInfo
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- CN211644817U CN211644817U CN201922159336.3U CN201922159336U CN211644817U CN 211644817 U CN211644817 U CN 211644817U CN 201922159336 U CN201922159336 U CN 201922159336U CN 211644817 U CN211644817 U CN 211644817U
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Abstract
The utility model provides a device for treating and recycling yellow phosphorus wastewater, wherein a phosphorus melting water tank is connected with a sedimentation tank, the sedimentation tank is connected with a condenser through a pump, the condenser is connected with a filter, and the filter is connected with a clean water tank; the clean water tank is connected to a matched water replenishing system through a pump. The sedimentation tank is formed by connecting a primary sedimentation tank, a secondary sedimentation tank and a tertiary sedimentation tank in series. The filter is connected with a phosphorus melting water pool. The cleaning water tank is also connected with a preheater through a pump, and the preheater is connected with a phosphorus melting water tank. The technical scheme of the utility model solve earlier in the yellow phosphorus production phosphorus trichloride in-process waste water carry out multistage settlement earlier with the waste water of heat preservation water seal yellow phosphorus and stew, make the free phosphorus of aquatic can obtain fully to stew and subside preseparation, can regard as the phosphorus pressing water used repeatedly of phosphorus trichloride production process, greatly reduced phosphorus trichloride production system instrument because of the problem of impurity jam. The amount of discharged wastewater is reduced by more than 60%.
Description
Technical Field
The utility model discloses a belong to yellow phosphorus waste water environmental protection cyclic utilization field, mainly solve the processing that the glyphosate enterprise wades phosphorus waste water at the use yellow phosphorus in-process, concretely relates to phosphorus waste water recycle's device and method. In particular to low-temperature membrane treatment filtration, three-stage sedimentation, clean water reuse in phosphorus trichloride production and hydrochloric acid recovery in the downstream dimethyl phosphite production process.
Background
Yellow phosphorus belongs to inflammable substances and is generally stored in a water-sealed barrel or stored in a water-sealed ground tank. At present, most domestic yellow phosphorus using enterprises store yellow phosphorus in a hot water melting mode in the aspect of yellow phosphorus storage. In related chemical enterprises taking yellow phosphorus as a production raw material, molten phosphorus wastewater is a main source of industrial wastewater, main pollutants are elemental phosphorus, free phosphorus and the like which cannot be fully utilized in water, and the molten phosphorus wastewater is characterized by soluble solids and large discharge amount. The treatment of the partial wastewater is difficult and the water quality is complex, and because the wastewater contains phosphorus in other forms, the toxicity of the wastewater is high, the influence on the environment is serious, and the discharge of the phosphorus-containing wastewater is strictly forbidden by an environment management department, so that the treatment of the yellow phosphorus wastewater needs to pay attention to the recycling in the development process of phosphorus-related enterprises.
When the traditional yellow phosphorus is used, hot water is needed for heat preservation and melting so as to isolate air and prevent spontaneous combustion. In recent years, because the consciousness of environmental protection is gradually improved, for yellow phosphorus wastewater, the management and control of each enterprise is more and more strict, but the generation of related wastewater cannot be avoided, most enterprises forbid or reduce wastewater discharge, but long-term closed use will cause the free phosphorus content in a molten phosphorus water system to be high, the water quality to be strong, and many foreign matters, which seriously affects the use of subsequent yellow phosphorus, for example, in a phosphorus trichloride production process, free phosphorus in yellow phosphorus wastewater, impurities block a flowmeter, cause the fluctuation of a production system, and seriously affect the intrinsic safety of a chlorination process.
Disclosure of Invention
The utility model discloses to the waste water of glyphosate enterprise in the yellow phosphorus use and manage comprehensively, provide a yellow phosphorus industrial waste water handles and cyclic utilization's device. The method mainly aims to carry out multistage standing sedimentation on the molten phosphorus water system, carry out sedimentation pre-separation on impurities accumulated in the long-term recycling process of a water body, enter a water quality purification system after separation, and enter a clean molten phosphorus water tank for independent storage after purification. Compared with the traditional production mode, the method has the advantages that firstly, impurities in the yellow phosphorus wastewater are reduced, and the stability of a subsequent production system is ensured. And secondly, one part of the hydrochloric acid is used for recovering and replenishing water, so that the regular water quality replacement can be realized, the water quality deterioration caused by long-term closed circulation is avoided, and the phosphorus resource can be deeply utilized in the downstream glyphosate synthesis process after the cyclic use.
A device for treating and recycling yellow phosphorus wastewater is characterized in that a phosphorus melting water tank is connected with a sedimentation tank, the sedimentation tank is connected with a condenser through a pump, the condenser is connected with a filter, and the filter is connected with a clean water tank; the clean water tank is connected to a matched water replenishing system through a pump.
The sedimentation tank is formed by connecting a primary sedimentation tank, a secondary sedimentation tank and a tertiary sedimentation tank in series.
The filter is connected with a phosphorus melting water pool. The cleaning water tank is also connected with a preheater through a pump, and the preheater is connected with a phosphorus melting water tank. The clean water tank is also connected with the filter through a pump.
The production equipment in melt the phosphorus pond and be equipped with the overflow mouth, and overflow mouth and one-level sedimentation tank intercommunication, one-level sedimentation tank is equipped with the overflow mouth, again with second grade sedimentation tank intercommunication, second grade sedimentation tank is equipped with the overflow mouth and communicates with tertiary sedimentation tank again, connect the condenser through waste water delivery pump behind the tertiary sedimentation tank, condenser waste water outlet is connected with the filter of phosphorus, the filter export is connected with the clean pond inlet pipeline of melting phosphorus, clean pond outlet pipeline is connected with the back flush pipeline of filter simultaneously. Meanwhile, the device can be connected with a preheater and then connected with a yellow phosphorus metering tank pressure phosphorus water tank in a phosphorus trichloride production device, and can also be connected with a water replenishing pipeline of a hydrochloric acid recovery water absorption tower in the dimethyl phosphite production process.
The phosphorus melting cleaning water tank is connected with the back flush of the filter, one part of the sewage drainage pipeline after cleaning is connected to the sewage treatment station, and the other part of the sewage drainage pipeline is connected to the phosphorus melting water tank.
The molten phosphorus water tank is conveyed to the first-level sedimentation tank, then the molten phosphorus water tank is conveyed to the second-level sedimentation tank and the third-level sedimentation tank through a water head overflow mode, the molten phosphorus water tank is conveyed to the condenser and the phosphorus filtering device through a centrifugal pump, and the backwashing process, the clean water pressure phosphorus water tank and the hydrochloric acid recovery system are both conveyed through the centrifugal pump.
The filtering device adopts a nanofiltration ceramic membrane for filtering, and because the yellow phosphorus wastewater belongs to low suspended solid load, bottom water inlet is recommended for the application of the low suspended solid load.
A process for recycling yellow phosphorus industrial wastewater after treatment mainly comprises index control of free phosphorus in molten phosphorus water, water turbidity control, filtering temperature and the like, and specifically comprises the following steps:
in the process of recycling treated yellow phosphorus industrial wastewater, the molten phosphorus water is ensured to be kept stand and settled as much as possible, the pH value of the molten phosphorus wastewater is ensured to be 3-8 as much as possible, the water temperature is controlled to be 30-70 ℃, the molten phosphorus water is gradually settled and overflowed, the molten phosphorus water is extracted from a three-stage settling tank through a centrifugal pump and is cooled by a condenser, the outlet temperature of materials of the condenser is controlled to be below 30 ℃, the condenser can be cooled by circulating water or frozen salt water (the temperature at the stage is not too low and is not lower than 10 ℃), and the cooled wastewater enters a filtering device to separate impurities such as free phosphorus and the like of the molten phosphorus water. After separation, indexes such as turbidity, total phosphorus, free phosphorus and the like of produced water are monitored, the average turbidity of the water in the phosphorus melting water pool before filtration is about 100NTU, the total phosphorus is about 300ppm, other forms such as free phosphorus are about 100ppm, the turbidity after filtration is reduced to be less than 2NTU, and other forms such as free phosphorus about 220ppm are reduced to be less than 2 ppm. When indexes such as turbidity, total phosphorus, free phosphorus and the like in the produced water are ultrahigh, the pressure of the filtering device rises, the quality of the produced water is deteriorated and cannot reach the use standard, at the moment, backwashing can be carried out by using clean water or medicaments, the cleaning time is generally 1-3min, and the backwashing can be specifically determined according to the pressure change condition of the filtering device.
One part of the clean water is used as phosphorus pressing water metered by yellow phosphorus in the phosphorus trichloride production process, the used phosphorus pressing water enters a phosphorus melting tank through a circulating pipeline and is continuously used after repeated circulating filtration, the other part of the clean water is filtered, because free phosphorus and other simple substance phosphorus in the water are basically filtered, part of total phosphorus still exists in the water, the average content of the total phosphorus in the hydrochloric acid is about 2000-4000ppm, the water can be applied to a hydrochloric acid recovery system of a coproduction glyphosate enterprise, on one hand, the intake of external water is reduced, and on the other hand, the phosphorus resource can be further effectively recovered and utilized.
The agent can be citric acid/hydrochloric acid chemical cleaning agent with pH of 1-2, and the cleaning frequency and time can be determined by the specific flux of the nanofiltration membrane.
In the preferred scheme, the multistage sedimentation standing pool is divided into three stages of sedimentation, and a reasonable grading mode can be specifically carried out according to the condition of water quality.
In a preferred scheme, the phosphorus filtering device can select a proper membrane device for filtering, a ceramic membrane is selected for filtering in the scheme, and the temperature before water inlet is lower than 30 DEG C
In the preferred scheme, the condenser adopts a tube-in-tube condenser, freezing saline water can be selected as a freezing medium in summer, circulating water can be selected for cooling in winter, and the temperature of water out of the condenser is required to be lower than 30 ℃.
In the preferred scheme, the clean water phosphorus trichloride removing production system is preheated before being used as phosphorus pressing water, a preheater can be preheated by high-temperature wastewater in a phosphorus melting system, and can also be directly heated by steam, and the heating steam has less oxygen content and various impurities and can be used as clean water supplement for production water.
In the preferred scheme, the clean water can be used as backwashing water of the phosphorus filtering device, and can also be externally accessed with new water (or medicament) for cleaning, if the clean water is used for cleaning, a small amount of cleaning wastewater enters the sewage treatment station, the subsequent cleaning can be determined according to the dirt degree of the filtering device, and the subsequent cleaning wastewater is collected to the phosphorus melting tank system for filtering and recycling again.
Advantageous effects
In the traditional process flow of enterprises for producing phosphorus trichloride by using yellow phosphorus, most of yellow phosphorus melting phosphorus wastewater is discharged after being treated, and as part of water is generally acidic, acid-base neutralization is carried out before treatment, and the pH value is adjusted to be neutral.
The new scheme is mechanically applied and optimized for the problem that yellow phosphorus wastewater is difficult to treat, firstly, the wastewater of the heat-preservation water sealed yellow phosphorus is subjected to multistage sedimentation and standing, free phosphorus in the water can be fully settled and settled for pre-separation, and then is subjected to further deep filtration through a phosphorus filtering device, although the purified water cannot reach the direct discharge standard, the purified water can be reused as phosphorus pressing water in the phosphorus trichloride production process, the problem of blockage of instruments of the phosphorus trichloride production system due to impurities is greatly reduced, the service life is greatly prolonged, the content of free phosphorus in the system is reduced, the safety risk during maintenance and replacement is reduced, and the intrinsic safety is improved. Meanwhile, the production amount of the wastewater is greatly reduced, the water is basically not required to be changed from the conventional regular water change to the present, and the amount of the discharged wastewater is reduced by more than 60%.
Meanwhile, clean water is further used for supplementing water for hydrochloric acid recovery by using a downstream process of co-production of glyphosate, so that introduction of new external water is reduced, the treatment cost of waste mother liquor in the production process of glyphosate is further reduced, water is saved from the source, emission is reduced, and economic and environmental-friendly benefits are remarkable.
Drawings
FIG. 1 shows a yellow phosphorus wastewater treatment and recycling device, 1. a phosphorus melting water tank (model: phi 4000 x 5000, stainless steel), 2-1. a primary sedimentation tank (model: 7600 x 2000, acid-resistant brick), 2-2. a secondary sedimentation tank (model: 5000 x 2000, acid-resistant brick), 2-3. a tertiary sedimentation tank (model: 5000 x 2000, acid-resistant brick), 3. a condenser (model: 316L,20m, etc.)3Tubular condenser)And 4. filter (model: Nanostone-CM-131TM high density one)Ceramic membrane integrated), 5. clean water tank (model: phi 4000 x 5000, stainless steel), 6-preheater (model: 316L,20m3Tubular condenser)。
Detailed Description
Example 1
A device for treating and recycling yellow phosphorus wastewater is characterized in that a phosphorus melting water tank 1 is connected with a sedimentation tank, the sedimentation tank is connected with a condenser 3 through a pump, the condenser 3 is connected with a filter 4, and the filter 4 is connected with a clean water tank 5; the cleaning water tank 5 is connected to a matched water replenishing system through a pump.
The sedimentation tank is formed by connecting a primary sedimentation tank 2-1, a secondary sedimentation tank 2-2 and a tertiary sedimentation tank 2-3 in series.
The filter 4 is connected with the molten phosphorus pool 1. The cleaning water tank 5 is also connected with a preheater 6 through a pump, and the preheater 6 is connected with the phosphorus melting water tank 1. The clean water basin 5 is also connected to the filter 4 via a pump.
Example 2
The process carried out using the apparatus of example 1 was as follows:
in the process of recycling treated industrial wastewater of yellow phosphorus, the molten phosphorus water is kept stand and settled as much as possible, the pH value of the molten phosphorus water is controlled between 3 and 8, the water temperature is controlled between 30 and 70 ℃, the molten phosphorus water is gradually settled and overflowed, the molten phosphorus water is extracted from a three-stage settling pond through a centrifugal pump and is cooled by a condenser, the outlet temperature of materials of the condenser is controlled below 30 ℃, the condenser is cooled by circulating water or frozen brine, one part of the clean water after cooling and filtering is used as phosphorus pressing water metered by yellow phosphorus in the production process of phosphorus trichloride, the used phosphorus pressing water enters a phosphorus melting tank through a circulating pipeline, and the like, the clean water is repeatedly filtered and recycled, and the other part of the clean water is filtered, and a downstream procedure of co-production of glyphosate is applied as water replenishing water for recycling of hydrochloric acid, so that the introduction of external new water is reduced.
Claims (5)
1. A device for treating and recycling yellow phosphorus wastewater is characterized in that a phosphorus melting water tank (1) is connected with a sedimentation tank, the sedimentation tank is connected with a condenser (3) through a pump, the condenser (3) is connected with a filter (4), and the filter (4) is connected with a cleaning water tank (5); the cleaning water tank (5) is connected to a matched water replenishing system through a pump.
2. The device for treating and recycling yellow phosphorus wastewater according to claim 1, wherein the sedimentation tank is formed by connecting a primary sedimentation tank (2-1), a secondary sedimentation tank (2-2) and a tertiary sedimentation tank (2-3) in series.
3. The apparatus for treating and recycling yellow phosphorus wastewater according to claim 2, wherein the filter (4) is connected to the pool (1) of molten phosphorus.
4. The apparatus for treating and recycling yellow phosphorus wastewater according to claim 3, wherein the cleaning water tank (5) is further connected with a preheater (6) through a pump, and the preheater (6) is connected with the phosphorus melting water tank (1).
5. The apparatus for treating and recycling yellow phosphorus wastewater according to claim 4, wherein the clean water tank (5) is further connected to the filter (4) via a pump.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201922159336.3U CN211644817U (en) | 2019-12-05 | 2019-12-05 | Yellow phosphorus wastewater treatment and cyclic utilization's device |
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| CN201922159336.3U CN211644817U (en) | 2019-12-05 | 2019-12-05 | Yellow phosphorus wastewater treatment and cyclic utilization's device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560545A (en) * | 2022-03-08 | 2022-05-31 | 贵州开阳青利天盟化工有限公司 | A waste water cyclic utilization system for in yellow phosphorus storage |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560545A (en) * | 2022-03-08 | 2022-05-31 | 贵州开阳青利天盟化工有限公司 | A waste water cyclic utilization system for in yellow phosphorus storage |
| CN114560545B (en) * | 2022-03-08 | 2023-10-03 | 贵州开阳青利天盟化工有限公司 | Wastewater recycling system for yellow phosphorus storage |
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