CN113816350A - Phosphoric acid recovery treatment process and system - Google Patents
Phosphoric acid recovery treatment process and system Download PDFInfo
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- CN113816350A CN113816350A CN202111029035.4A CN202111029035A CN113816350A CN 113816350 A CN113816350 A CN 113816350A CN 202111029035 A CN202111029035 A CN 202111029035A CN 113816350 A CN113816350 A CN 113816350A
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 314
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 157
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000011084 recovery Methods 0.000 title claims abstract description 43
- 239000002699 waste material Substances 0.000 claims abstract description 67
- 238000004140 cleaning Methods 0.000 claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 52
- 238000000746 purification Methods 0.000 claims abstract description 30
- 238000005406 washing Methods 0.000 claims abstract description 29
- 239000013043 chemical agent Substances 0.000 claims abstract description 21
- 239000010865 sewage Substances 0.000 claims abstract description 15
- 239000012535 impurity Substances 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims description 62
- 239000002253 acid Substances 0.000 claims description 57
- 238000011010 flushing procedure Methods 0.000 claims description 49
- 238000005371 permeation separation Methods 0.000 claims description 42
- 238000001914 filtration Methods 0.000 claims description 11
- 244000005700 microbiome Species 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 9
- 239000003814 drug Substances 0.000 claims description 8
- 239000000084 colloidal system Substances 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 230000001954 sterilising effect Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 abstract description 16
- 239000011888 foil Substances 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 230000015572 biosynthetic process Effects 0.000 abstract description 11
- 239000003990 capacitor Substances 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000007667 floating Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- QVLTXCYWHPZMCA-UHFFFAOYSA-N po4-po4 Chemical compound OP(O)(O)=O.OP(O)(O)=O QVLTXCYWHPZMCA-UHFFFAOYSA-N 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- 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
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a phosphoric acid recovery treatment process for overcoming the problem of higher use cost and treatment cost of phosphoric acid in the formation process of a capacitor aluminum foil in the prior art, which comprises a phosphoric acid purification process, a chemical agent washing process and a self-washing process. The invention also discloses a phosphoric acid recovery processing system, which comprises a phosphoric acid purification unit, a cleaning unit and a pure water supply unit. The invention provides a phosphoric acid recovery treatment process which is simple, can reduce the impurity content in phosphoric acid waste liquid, realizes phosphoric acid recovery and utilization, and has a recovery rate of 50-60%. The invention also provides a phosphoric acid recovery processing system, which can recover a large amount of phosphoric acid for the aluminum foil formation production, saves the phosphoric acid and reduces the production cost. Meanwhile, the phosphoric acid content in the concentrated water is reduced, so that the requirement on sewage station equipment is reduced, and the treatment cost of a subsequent sewage treatment station is also reduced.
Description
Technical Field
The invention relates to the field of capacitor aluminum foil production technology, in particular to a phosphoric acid recovery treatment process and system in capacitor aluminum foil production.
Background
The low-pressure aluminum foil for aluminum electrolytic capacitor is treated with phosphoric acid during the formation process, so as to raise the specific volume of aluminum foil and improve the structure characteristic of aluminum oxide film. Therefore, the using amount of phosphoric acid in the formation of the capacitor aluminum foil is large, and the cost is higher.
On the other hand, the content of impurities in the formed phosphoric acid is gradually increased until the phosphoric acid is not used for production. The waste phosphoric acid can not be directly discharged, and needs to be collected to a sewage station for industrial wastewater treatment, so that the treatment cost is higher.
Disclosure of Invention
The invention provides a phosphoric acid recovery treatment process for overcoming the problem that the use cost and the treatment cost of phosphoric acid are high in the formation process of capacitor aluminum foil in the prior art, the process is simple, the impurity content in phosphoric acid waste liquid can be reduced, the phosphoric acid is recycled, and the recovery rate is 50-60%.
The invention also provides a phosphoric acid recovery processing system, which can recover a large amount of phosphoric acid for the aluminum foil formation production, saves the phosphoric acid and reduces the production cost. Meanwhile, the phosphoric acid content in the concentrated water is reduced, so that the requirement on sewage station equipment is reduced, and the treatment cost of a subsequent sewage treatment station is also reduced.
And a system for the same, and a method for the same,
the technical scheme adopted by the invention is as follows:
the phosphoric acid recovery treatment process comprises a phosphoric acid purification process, a chemical agent washing process and a self-washing process;
the phosphoric acid purification process is used for phosphoric acid purification, and the main process flow is as follows:
step 1, collecting phosphoric acid waste liquid and sterilizing;
step 2, filtering the phosphoric acid waste liquid, and separating suspended matters, precipitates, microorganisms, colloids and the like;
3, pressurizing, separating the phosphoric acid waste liquid by adopting membrane permeation separation equipment to obtain phosphoric acid with low impurity content, reusing the phosphoric acid, and discharging concentrated water to a sewage station for treatment;
the chemical agent flushing process is used for cleaning the permeation separation equipment, and the main process flow is as follows:
step 1, stopping a phosphoric acid extraction process flow, and injecting a cleaning liquid medicine into a permeation separation device;
step 2, discharging the cleaning liquid from the filtration membrane permeation separation equipment, injecting the separation liquid into the membrane permeation separation equipment again for cleaning, and discharging the cleaning liquid after circularly cleaning for 0.5-2 hours;
step 3, injecting pure water into the permeation separation equipment, stopping the chemical agent washing process flow after cleaning is finished, and switching to a phosphoric acid purification process flow;
the self-flushing process and the phosphoric acid purification process are carried out synchronously and are used for cleaning the permeation separation equipment, and the main process flow is as follows:
step 1, stopping phosphoric acid collection and concentrated water discharge, directly flushing the membrane permeation separation equipment with waste phosphoric acid under pressure, and refluxing washing liquor to the phosphoric acid waste liquor for treatment.
A phosphoric acid recovery processing system comprises
A phosphoric acid purification unit having a membrane permeation separation apparatus;
the cleaning unit is communicated with the membrane permeation separation equipment and is used for cleaning the membrane permeation separation equipment by chemical agents or self-flushing the membrane permeation separation equipment;
and a pure water supply unit for supplying pure water to the phosphoric acid purification unit and the cleaning unit.
Further, the phosphoric acid treatment unit comprises
A spent acid collection tank having an overflow tube and a first level gauge;
the lifting pump is provided with a second valve and a first check valve, and the input front end of the lifting pump is communicated with the waste acid collecting box;
a filter having a fourth valve, a second pressure sensor and a first temperature sensor, an input front end of which communicates with an output end of the lift pump;
a high pressure pump having a fifth valve, a sixth valve and a second check valve, an input front end of which communicates with an output end of the filter;
the membrane permeation separation equipment is provided with a tubular membrane filter, a concentrated water pipeline, an acid liquor pipeline and an external circulation pipeline; the input front end of the tubular membrane filter is communicated with the output tail end of the high-pressure pump; one end of the external circulation pipeline is communicated with the concentrated water pipeline, and the other end of the external circulation pipeline is communicated with the input front end of the tubular membrane filter;
and the acid recovery tank is provided with a liquid level meter and a recycling pump and is communicated with the output tail end of the acid liquor pipeline.
Further, also includes
The bypass pipeline is provided with a third valve, and two ends of the bypass pipeline are respectively communicated with the input front end and the output tail end of the lifting pump;
a flow meter having a first pressure sensor with an input front end in communication with an output end of the lift pump and an output end in communication with the filtered input front end.
Further, also includes
The first degerming device is arranged in the waste acid collecting box;
and the second degerming device is arranged in the acid recovery box.
Further, also includes
The sixth valve is arranged on the concentrated water pipeline;
a seventh valve disposed on the acid liquid line;
and the eighth valve, the circulating pump, the ninth valve and the third check valve are arranged on the external circulating pipeline.
Further, the cleaning unit comprises
The medicament flushing mechanism is communicated with the concentrated water pipeline, the acid liquor pipeline and the external circulation pipeline;
and the input front end of the self-flushing pipeline is communicated with the tubular membrane filter and is provided with an electric valve, and the output tail end of the self-flushing pipeline is connected to the waste acid collecting box.
Further, the medicament flushing mechanism comprises
A cleaning box is arranged at the bottom of the tank,
a flushing liquid inlet pipeline which is provided with a tenth valve, a Y-shaped filter and an eleventh valve, wherein one end of the flushing liquid inlet pipeline is communicated with the cleaning tank, and the other end of the flushing liquid inlet pipeline is communicated with the input front end of the circulating pump;
and the parallel input front ends of the flushing and drainage pipelines are respectively communicated with the concentrated water pipeline and the acid liquor pipeline, a tenth valve and a tenth valve are respectively arranged on the flushing and drainage pipelines, and the parallel output tail ends of the flushing and drainage pipelines are converged and communicated with the cleaning tank and provided with a fourteenth valve and a drainage valve.
Further, the pure water replenishment unit 100 injects pure water into the waste acid collection tank, the recovered acid tank, and the cleaning tank, and is provided with a fifteenth valve, a sixteenth valve, and a seventeenth valve, respectively.
The invention has the beneficial effects that:
1. the invention provides a phosphoric acid recovery treatment process for improving the utilization rate of phosphoric acid and solving the problem of higher use cost and treatment cost of phosphoric acid in the formation process of a capacitor aluminum foil. The process is simple, the impurity content in the phosphoric acid waste liquid can be reduced, the phosphoric acid is recycled, the recovery rate is 50-60%, and the production cost and the treatment cost are reduced.
2. The invention also provides a phosphoric acid recovery processing system, which comprises a phosphoric acid purification unit, a cleaning unit and a pure water supply unit. The phosphoric acid purification unit is provided with a membrane permeation separation device; the cleaning unit is communicated with the membrane permeation separation equipment and is used for cleaning the membrane permeation separation equipment by chemical agents or self-flushing the membrane permeation separation equipment; the pure water supply unit supplies pure water to the phosphoric acid purification unit and the cleaning unit. The system can recover a large amount of phosphoric acid and reuse the phosphoric acid for the aluminum foil formation production, thereby saving the phosphoric acid and reducing the production cost. Meanwhile, the phosphoric acid content in the concentrated water is reduced, so that the requirement on sewage station equipment is reduced, and the treatment cost of a subsequent sewage treatment station is also reduced.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of a phosphoric acid recovery processing system in an embodiment.
Detailed Description
In the following, only certain exemplary embodiments are briefly described. As those skilled in the art will recognize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature, and not as restrictive.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
The following disclosure provides many different embodiments or examples for implementing different features of the invention. To simplify the disclosure of the present invention, the components and arrangements of specific examples are described below. Of course, they are merely examples and are not intended to limit the present invention.
Embodiments of the invention are described in detail below with reference to the accompanying drawings.
In this embodiment, in order to improve the utilization rate of phosphoric acid and solve the problem that the use cost and the treatment cost of phosphoric acid are high in the formation process of the capacitor aluminum foil, a phosphoric acid recovery treatment process is provided, which includes a phosphoric acid purification process, a chemical agent flushing process and a self-flushing process, and the chemical agent flushing process and the self-flushing process are not adopted at the same time.
The phosphoric acid purification process is mainly used for phosphoric acid purification, and comprises the following process flows:
step 1, collecting phosphoric acid waste liquid and sterilizing;
step 2, filtering the phosphoric acid waste liquid, and separating suspended matters, precipitates, microorganisms, colloids and the like;
and 3, pressurizing, separating the phosphoric acid waste liquid by adopting membrane permeation separation equipment to obtain phosphoric acid with low impurity content, reusing the phosphoric acid, and discharging concentrated water to a sewage station for treatment.
The chemical agent flushing process is mainly used for cleaning the permeation separation equipment and comprises the following process flows:
step 1, stopping a phosphoric acid extraction process flow, and injecting a cleaning liquid medicine into a permeation separation device;
step 2, discharging the cleaning liquid from the filtration membrane permeation separation equipment, injecting the separation liquid into the membrane permeation separation equipment again for cleaning, and discharging the cleaning liquid after circularly cleaning for 0.5-2 hours;
and 3, injecting pure water into the permeation separation equipment, stopping the chemical agent washing process flow after cleaning is finished, and switching to a phosphoric acid purification process flow.
The self-flushing process is synchronous with the phosphoric acid purification process, is mainly used for cleaning the permeation separation equipment, and comprises the following process flows:
step 1, stopping phosphoric acid collection and concentrated water discharge, directly flushing the membrane permeation separation equipment with waste phosphoric acid under pressure, and refluxing washing liquor to the phosphoric acid waste liquor for treatment.
In the embodiment, a phosphoric acid recovery processing system is also provided, as shown in fig. 1. The system comprises a phosphoric acid purification unit, a cleaning unit and a pure water supply unit.
Specifically, the phosphoric acid purification unit comprises a waste acid collecting tank 10, a lift pump 20, a flow meter 30, a filter 40, a high-pressure pump 50, a membrane permeation separation device 60 and a recovered acid tank 70.
The waste acid collecting box 10 is provided with a waste acid liquid inlet pipe 11, a first liquid level meter 12, an overflow pipe 13 and a first degerming device 14. The waste acid liquid inlet pipe 11 is used for guiding waste phosphoric acid generated on an aluminum foil production line into the waste acid collecting box 1. The first level gauge 12 is used for monitoring the liquid level height in the waste acid collecting tank 1. When the liquid level in the waste acid collecting box 1 exceeds the limit, the over-limit waste phosphoric acid is discharged to the sewage treatment station through the overflow pipe 13. The first sterilizer 14 is installed in the waste acid collecting box 10, for example, an ultraviolet lamp is used to kill microorganisms, bacteria, etc. in the waste phosphoric acid, and reduce the influence of the microorganisms, bacteria, etc. on the subsequent treatment process.
And the lifting pump 20 is connected with the waste acid collecting box 1, and is used for pumping out the waste phosphoric acid in the waste phosphoric acid collecting box 1 and lifting the height of the waste phosphoric acid liquid. The input front end of the lift pump 20 is connected to the waste acid collecting tank 1 and is provided with a first valve 21, and the output end of the lift pump 20 is provided with a second valve 22 and a first check valve 23. The first check valve 23 allows the waste phosphoric acid pumped by the lift pump 20 to flow only in one direction toward the next process. A bypass line 24 is provided outside the lift pump 20 to allow the waste phosphoric acid pumped by the lift pump 20 to partially flow back. The bypass line 24 has one end communicating with the input front end of the lift pump 20 and the other end communicating with the output end of the first check valve 22, and is installed with a third valve 241.
And the flow meter 30 is communicated with the output tail end of the first check valve 22 at the input front end and is used for adjusting and/or displaying the amount of the waste phosphoric acid pumped to the next process by the current lifting pump 20. When the flow meter 30 has the adjusting function, if the pumping amount of the lift pump 20 is larger than the control amount of the flow meter 30, the third valve 23 is in the open state, and the part of the waste phosphoric acid pumped by the lift pump 20 flows back through the bypass line. A first pressure sensor 31 is provided at the output end of the flow meter 30 to monitor the real-time pressure in the pipe.
And a filter 40 whose upper portion communicates with an output end of the flowmeter 30. The filter 40 is a security filter, a vertical column-shaped device is internally provided with a polypropylene melt-blown filter element or a wire-wound filter element, the working principle is that the filter element pores are utilized for mechanical filtration, water passes through the tiny micropores of the filter element, and residual trace suspended particles, colloid, microorganisms and the like in the water are intercepted or adsorbed on the surface and in the pores of the filter element, and the capability of intercepting impurities is mainly determined by the pore diameter of the filter element, so that the filter is suitable for deep purification of water with lower suspended impurities. The filter 40 is vented at the top and the bottom is vented of the separated floating particles, colloids, microorganisms, etc. The spent phosphoric acid is introduced from the upper portion of the filter 40 after being raised by the lift pump 20, and the separated phosphoric acid is discharged from the lower portion of the filter 40. The output end of the filter 40 is mounted with a fourth valve 41, a second pressure sensor 42, and a first temperature sensor 43. The second pressure sensor 42 and the first temperature sensor 43 are used to monitor the pressure and temperature of the phosphoric acid in the tube after being filtered by the filter 40, respectively.
And a high-pressure pump 50 whose input front end communicates with the output end of the filter 40. A fifth valve 51 is installed at an input front end of the high-pressure pump 50, and a sixth valve 52 and a second check valve 53 are installed at an output end of the high-pressure pump 50. The waste phosphoric acid pumped by the high pressure pump 50 is allowed to flow to the next process only in one direction.
And a membrane permeation separation device 60 communicating with an output end of the high-pressure pump 50. The membrane permeation separation device 60 includes a tubular membrane filter 61, a concentrated water line 62, an acid liquid line 63, and an external circulation line 64. One or more ceramic tube membranes are provided within the tube membrane filter 61. A sixth valve 621 is provided on the concentrate line 62. A seventh valve 631 is provided in the acid line 63. The external circulation line 64 has one end communicating with the concentrate line 62 and the other end communicating with the input front end of the tubular membrane filter 61, and is provided with an eighth valve 641, a circulation pump 642, a ninth valve 643, and a third check valve 644. The output end of the high-pressure pump 50 is communicated with a tubular membrane filter 61, waste phosphoric acid passes through the ceramic tubular membrane, phosphoric acid with low impurity content passes through the pores of the ceramic tubular membrane to obtain phosphoric acid and is collected into an acid liquor pipeline 63, and impurities and the like are intercepted and collected into a concentrated water pipeline 62. Part of the concentrated water in the concentrated water pipeline 62 is sent to a sewage station for treatment, and part of the concentrated water is pumped by the circulating pump 642 and flows back to the tubular membrane filter 61 again for membrane permeation filtration.
And the acid recovery tank 70 is communicated with the output tail end of the acid liquid pipeline 63. The recovered acid tank 70 is provided with a second liquid level meter 71, a second sterilizer 72 and a recycling pump 73. The second level meter 71 is used to monitor the level of the phosphoric acid recovered in the recovered acid tank 70. The second sterilizer 72 is installed in the recovered acid tank 70, for example, an ultraviolet lamp is used to kill microorganisms, bacteria, etc. in the waste phosphoric acid, and reduce the influence of the microorganisms, bacteria, etc. on the subsequent processes. The recycling pump 73 is communicated with the lower part of the outer side of the recycling acid tank 70 and can be pumped back to the capacitor aluminum foil formation production line for use.
The cleaning unit includes a medicament flushing mechanism 80 and a self-flushing line 90.
And the medicament flushing mechanism 80 is communicated with the concentrated water pipeline 62, the acid liquor pipeline 63 and the external circulation pipeline 64. The flushing mechanism 80 includes a cleaning tank 81, a flushing inlet line 82, and a flushing outlet line 83. The flushing liquid inlet pipeline 82 is communicated with the cleaning tank 81 at one end and the input front end of the circulating pump 642 at the other end, and comprises a tenth valve 821, a Y-shaped filter 822 and an eleventh valve 823. The flushing drainage pipeline 83 is a parallel pipeline, the parallel input front end of the flushing drainage pipeline is respectively communicated with the concentrated water pipeline 62 and the acid liquor pipeline 63, and a tenth valve 831 and a thirteenth valve 832 are respectively installed on the flushing drainage pipeline. The flushing drain line 83 is connected in parallel and connected to the outlet end and connected to the cleaning tank 81, and a fourteenth valve 833 and a drain valve 834 are installed. When the tubular membrane filter 61 is cleaned with a chemical, the chemical is dissolved in the cleaning tank 81, and the undissolved portion is filtered and separated by the Y-filter 822. The chemical agent solution is pumped into the tubular membrane filter 61 through the circulating pump 642 to clean the ceramic tubular membrane, the cleaning solution is collected and flows back to the cleaning box 81, and the cleaning solution is cleaned again after being filtered through the Y-shaped filter 822. After washing for a period of time, the washing liquid stops flowing back into the washing tank 81 and is directly discharged.
The self-flushing pipeline 90 is communicated with the tubular membrane filter 61 at the input front end and is provided with an electric valve 91, and the output tail end is connected to the waste acid collecting box 10. The waste phosphoric acid stock solution is used for washing from the tubular membrane filter 61, and the washing solution flows back to the waste acid collecting box 10.
The pure water supply unit 100 injects pure water into the waste acid collection tank 10, the recovered acid tank 70, and the cleaning tank 81, and is provided with a fifteenth valve 110, a sixteenth valve 120, and a seventeenth valve 130, respectively.
Based on the phosphoric acid recovery processing system in the embodiment, the phosphoric acid recovery processing flow is as follows:
the phosphoric acid purification process flow comprises:
when phosphoric acid is purified, chemical agent washing and self-washing are not carried out.
The first valve 21, the second valve 22, the third valve 241, the fourth valve 41, the fifth valve 51, the sixth valve 52, the sixth valve 621, the seventh valve 631, the eighth valve 641, and the ninth valve 643 are opened, and the remaining valves are closed. The high-pressure pump 50 is started first, and then the circulation pump 642 is started. After the phosphoric acid waste liquid in the waste acid collecting tank 10 is lifted by the lift pump 20, the phosphoric acid waste liquid enters the filter 40 according to the flow set by the flow meter 30, and floating particles, colloids, microorganisms and the like are filtered. The separated waste phosphoric acid is pressurized by the high-pressure pump 50 and then injected into the tubular membrane filter 61. The waste phosphoric acid passes through the ceramic tube membrane, the phosphoric acid passes through the pores of the ceramic tube membrane to obtain the phosphoric acid with low impurity content, the phosphoric acid is collected into the acid liquor pipeline 63 and finally flows into the acid recovery tank 70, and impurities and the like are intercepted and collected into the concentrated water pipeline 62. Part of the concentrated water in the concentrated water pipeline 62 is sent to a sewage station for treatment, and part of the concentrated water is pumped by the circulating pump 642 and flows back to the tubular membrane filter 61 again for membrane permeation filtration.
The chemical agent washing process flow comprises the following steps:
when the chemical agent is washed, phosphoric acid purification and automatic washing are not carried out.
After the chemical is dissolved in the cleaning tank 81, an undissolved portion is filtered and separated by a Y-filter 822. The chemical agent solution is pumped into the tubular membrane filter 61 through the circulating pump 642 to clean the ceramic tubular membrane, the cleaning solution is collected and flows back to the cleaning box 81, and the cleaning solution is cleaned again after being filtered through the Y-shaped filter 822. After washing for a period of time, the washing liquid stops flowing back into the washing tank 81 and is directly discharged. After the cleaning cycle is carried out for 0.5-2 h, the fourteenth valve 833 is closed, and the drain valve 834 and the seventeenth valve 130 are opened. Pure water is injected into the cleaning tank 81. The pure water is pumped into the tubular membrane filter 61 through the circulation pump 642, and the pure water washing is continued until the chemical agent is washed clean.
The self-flushing process flow comprises the following steps:
when the self-washing is carried out, the purification of the phosphoric acid is not suspended and the washing of chemical agents is not carried out.
The first valve 21, the second valve 22, the third valve 241, the fourth valve 41, the fifth valve 51, the sixth valve 52, the eighth valve 641, the ninth valve 643 and the electric valve 91 are opened, and the remaining valves are closed.
After the phosphoric acid waste liquid in the waste acid collecting tank 10 is lifted by the lift pump 20, the phosphoric acid waste liquid enters the filter 40 according to the flow set by the flow meter 30, and floating particles, colloids, microorganisms and the like are filtered. The separated waste phosphoric acid is pressurized by the high-pressure pump 50 and then injected into the tubular membrane filter 61. The waste phosphoric acid stock solution is used for washing from the tubular membrane filter 61, and the washing solution flows back to the waste acid collecting box 10.
After the phosphoric acid is recovered by using the phosphoric acid recovery processing system in this embodiment, if the following table 1 is used for detection,
TABLE 1
| Phosphoric acid waste liquid discharged from workshop | Recovered phosphoric acid | |
| Phosphoric acid content | 2.28％ | 3.94％ |
| Electrical conductivity of | 23100us/cm | 27500us/cm |
| pH value | 1.45 | 1.43 |
It can be seen from table 1 that the phosphoric acid waste liquid after being recovered and treated has increased phosphoric acid content and increased conductivity, and the main reason is that the impurity content is reduced after being subjected to coarse filtration by a filter and fine filtration by a membrane permeation separation device, so as to meet the requirement of repeated use.
After the phosphoric acid recovery processing system in this example was continuously operated for a certain period of time, the phosphoric acid recovery rate was as shown in table 2 below,
TABLE 2
As can be seen from Table 2, the recovery rate of phosphoric acid recovered by the phosphoric acid recovery processing system in this embodiment is maintained at 50-60%, and can reach 65% at most. By adopting the phosphoric acid recovery processing system in the implementation, a large amount of phosphoric acid can be recovered and reused for aluminum foil formation production, so that the phosphoric acid is saved, and the production cost is reduced. Meanwhile, the phosphoric acid content in the concentrated water is reduced, so that the requirement on sewage station equipment is reduced, and the treatment cost of a subsequent sewage treatment station is also reduced.
Claims (9)
1. The phosphoric acid recovery treatment process is characterized by comprising a phosphoric acid purification process, a chemical agent washing process and a self-washing process;
the phosphoric acid purification process is used for phosphoric acid purification, and the main process flow is as follows:
step 1, collecting phosphoric acid waste liquid and sterilizing;
step 2, filtering the phosphoric acid waste liquid, and separating suspended matters, precipitates, microorganisms, colloids and the like;
3, pressurizing, separating the phosphoric acid waste liquid by adopting membrane permeation separation equipment to obtain phosphoric acid with low impurity content, reusing the phosphoric acid, and discharging concentrated water to a sewage station for treatment;
the chemical agent flushing process is used for cleaning the permeation separation equipment, and the main process flow is as follows:
step 1, stopping a phosphoric acid extraction process flow, and injecting a cleaning liquid medicine into a permeation separation device;
step 2, discharging the cleaning liquid from the filtration membrane permeation separation equipment, injecting the separation liquid into the membrane permeation separation equipment again for cleaning, and discharging the cleaning liquid after circularly cleaning for 0.5-2 hours;
step 3, injecting pure water into the permeation separation equipment, stopping the chemical agent washing process flow after cleaning is finished, and switching to a phosphoric acid purification process flow;
the self-flushing process and the phosphoric acid purification process are carried out synchronously and are used for cleaning the permeation separation equipment, and the main process flow is as follows:
step 1, stopping phosphoric acid collection and concentrated water discharge, directly flushing the membrane permeation separation equipment with waste phosphoric acid under pressure, and refluxing washing liquor to the phosphoric acid waste liquor for treatment.
2. The phosphoric acid recovery processing system is characterized by comprising
A phosphoric acid purification unit having a membrane permeation separation apparatus;
the cleaning unit is communicated with the membrane permeation separation equipment and is used for cleaning the membrane permeation separation equipment by chemical agents or self-flushing the membrane permeation separation equipment;
and a pure water supply unit for supplying pure water to the phosphoric acid purification unit and the cleaning unit.
3. The phosphoric acid recovery processing system of claim 2, wherein the phosphoric acid processing unit comprises
A spent acid collection tank having an overflow tube and a first level gauge;
the lifting pump is provided with a second valve and a first check valve, and the input front end of the lifting pump is communicated with the waste acid collecting box;
a filter having a fourth valve, a second pressure sensor and a first temperature sensor, an input front end of which communicates with an output end of the lift pump;
a high pressure pump having a fifth valve, a sixth valve and a second check valve, an input front end of which communicates with an output end of the filter;
the membrane permeation separation equipment is provided with a tubular membrane filter, a concentrated water pipeline, an acid liquor pipeline and an external circulation pipeline; the input front end of the tubular membrane filter is communicated with the output tail end of the high-pressure pump; one end of the external circulation pipeline is communicated with the concentrated water pipeline, and the other end of the external circulation pipeline is communicated with the input front end of the tubular membrane filter;
and the acid recovery tank is provided with a liquid level meter and a recycling pump and is communicated with the output tail end of the acid liquor pipeline.
4. The phosphoric acid recovery processing system of claim 3, further comprising
The bypass pipeline is provided with a third valve, and two ends of the bypass pipeline are respectively communicated with the input front end and the output tail end of the lifting pump;
a flow meter having a first pressure sensor with an input front end in communication with an output end of the lift pump and an output end in communication with the filtered input front end.
5. The phosphoric acid recovery processing system of claim 3, further comprising
The first degerming device is arranged in the waste acid collecting box;
and the second degerming device is arranged in the acid recovery box.
6. The phosphoric acid recovery processing system of claim 3, further comprising
The sixth valve is arranged on the concentrated water pipeline;
a seventh valve disposed on the acid liquid line;
and the eighth valve, the circulating pump, the ninth valve and the third check valve are arranged on the external circulating pipeline.
7. The phosphoric acid recovery processing system of any one of claim 6, wherein the cleaning unit comprises
The medicament flushing mechanism is communicated with the concentrated water pipeline, the acid liquor pipeline and the external circulation pipeline;
and the input front end of the self-flushing pipeline is communicated with the tubular membrane filter and is provided with an electric valve, and the output tail end of the self-flushing pipeline is connected to the waste acid collecting box.
8. The phosphoric acid recovery processing system of claim 7, wherein the agent flushing mechanism comprises
A cleaning box is arranged at the bottom of the tank,
a flushing liquid inlet pipeline which is provided with a tenth valve, a Y-shaped filter and an eleventh valve, wherein one end of the flushing liquid inlet pipeline is communicated with the cleaning tank, and the other end of the flushing liquid inlet pipeline is communicated with the input front end of the circulating pump;
and the parallel input front ends of the flushing and drainage pipelines are respectively communicated with the concentrated water pipeline and the acid liquor pipeline, a tenth valve and a tenth valve are respectively arranged on the flushing and drainage pipelines, and the parallel output tail ends of the flushing and drainage pipelines are converged and communicated with the cleaning tank and provided with a fourteenth valve and a drainage valve.
9. The phosphoric acid recovery processing system according to claim 3, wherein the pure water replenishment unit 100 injects pure water to the waste acid collection tank, the recovered acid tank and the cleaning tank, and is provided with a fifteenth valve, a sixteenth valve and a seventeenth valve, respectively.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111029035.4A CN113816350A (en) | 2021-09-02 | 2021-09-02 | Phosphoric acid recovery treatment process and system |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111029035.4A CN113816350A (en) | 2021-09-02 | 2021-09-02 | Phosphoric acid recovery treatment process and system |
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Application publication date: 20211221 |