CN112299635A - Method for purifying chemical polishing waste liquid - Google Patents
Method for purifying chemical polishing waste liquid Download PDFInfo
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- CN112299635A CN112299635A CN202011139595.0A CN202011139595A CN112299635A CN 112299635 A CN112299635 A CN 112299635A CN 202011139595 A CN202011139595 A CN 202011139595A CN 112299635 A CN112299635 A CN 112299635A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a method for purifying and treating chemical polishing waste liquid, which can fundamentally solve the problem of waste liquid treatment in the chemical polishing industry and reduce the sewage treatment cost and hazardous waste treatment cost of enterprises; the mode of the purification treatment of the chemical polishing waste liquid can control continuous operation, saves manpower, avoids the danger of manual operation of concentrated acid, has low operation energy consumption, has an extraction rate of 80-85 percent, is favorable for lightening the burden of an enterprise, has higher environmental protection value, is favorable for the development of the enterprise, and is worthy of popularization.
Description
Technical Field
The invention relates to the field of waste liquid treatment, in particular to a purification treatment mode of chemical polishing waste liquid.
Background
Chemical polishing is a method for eliminating grinding marks and etching and leveling by the selective dissolution of chemical etching of chemical reagents on uneven areas on the surface of a sample. The polishing method using the chemical solution has the advantages of simple equipment, capability of treating thin pipes, deep holes and parts with complex shapes and improvement of production efficiency, and one of the defects is that the service life of the used polishing solution is short, and the adjustment and regeneration of the solution concentration are difficult.
The commonly used chemical polishing solution is a two-acid or three-acid solution, and the two-acid chemical polishing solution has the following general components: 50-70% of 85% wt concentrated phosphoric acid and 30-50% of 98% wt concentrated sulfuric acid; the three-acid chemical polishing solution comprises the following components in percentage by weight: 60-70% of 85% wt concentrated phosphoric acid, 20-30% of 98% wt concentrated sulfuric acid and 5-10% of 75% wt concentrated nitric acid.
In the continuous use process of the polishing solution, the polishing effect of the polishing solution is gradually deteriorated due to the continuous dissolution of metal parts, the consumption of hydrogen ions and the continuous increase of the concentration of metal ions such as aluminum, iron and the like, and the polishing solution is called chemical polishing aging solution. The general treatment mode of the chemical polishing and aging solution is to discharge a part of the chemical polishing and aging solution and supplement fresh acid in proportion to ensure that the chemical polishing and aging solution meets the process requirements. The discharged chemical polishing and aging liquid is mixed concentrated acid waste liquid with high concentration of metal ions such as aluminum, iron and the like and acid radical ions. At the same time, the polished metal part surface will also carry a portion of the polishing solution, and thus the rinsing water will also be mixed with the polishing solution. The chemical polishing aging liquid is combined with multi-stage countercurrent rinsing water to be called chemical polishing waste liquid. At present, the chemical polishing waste liquid is lack of an effective recycling method, the cost is high when the chemical polishing waste liquid is treated by qualified hazardous waste treatment units, and if the chemical polishing waste liquid is used as waste water to be treated in a sewage station, a large amount of alkali is consumed and a large amount of sludge is generated, so that the cost of chemicals is high, and the cost of acid liquid is wasted.
The existing treatment mode of chemical waste liquid disposal faces the problems of low recovery rate or higher equipment investment and operation cost, so the key of the invention is to develop a purification mode which can effectively recycle valuable components in the waste liquid and reduce the comprehensive cost.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a mode for purifying chemical polishing waste liquid, which comprises the following steps: performing multistage countercurrent extraction by using a multistage countercurrent extraction device, feeding an organic phase extraction solvent into a multistage countercurrent extraction mechanism from a light phase inlet, feeding chemical polishing waste liquid into the multistage countercurrent extraction mechanism from a heavy phase inlet, starting a stirrer, driving the stirrer to operate to drive the organic phase extraction solvent and the chemical polishing waste liquid to be uniformly mixed in a mixing zone, contacting the organic phase extraction solvent and the chemical polishing waste liquid in the multistage countercurrent extraction mechanism, extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent, and standing and layering in a standing zone to obtain a loaded organic phase and a raffinate phase; the loaded organic phase is positioned on the upper layer of the raffinate phase, in the liquid separation zone, the raffinate phase flows to the mixing zone of the next extraction unit from the heavy phase inlet to the heavy phase outlet from a gap below the heavy phase limiting right-angle plate, and the loaded organic phase overflows from the upper part of the light phase overflow inclined plate to the mixing zone of the next extraction unit from the light phase inlet to the light phase outlet; the closer the loaded organic phase is to the heavy phase inlet, the higher the content of the mixed acid in the raffinate phase is, so that more and more loaded organic phases are discharged from the light phase outlet after further extraction; the more the raffinate phase is close to the light phase inlet, the higher the content of the organic phase extraction solvent in the loaded organic phase is, so that after further extraction, the content of the mixed acid in the raffinate phase is less and less, and finally the raffinate phase is discharged to a sewage treatment system from a heavy phase outlet, and the problems of low recovery rate or high equipment investment and operation cost in the conventional chemical waste liquid disposal mode are solved.
The purpose of the invention can be realized by the following technical scheme:
a method for purifying chemical polishing waste liquid comprises the following steps:
step one, collection: mixing chemical polishing aging liquid in a chemical polishing tank with rinsing water from a multistage countercurrent rinsing tank, and filtering the mixture in a chemical polishing waste liquid collecting tank through a bag filter to obtain chemical polishing waste liquid;
step two, extraction: in an extraction tank, contacting the chemical polishing waste liquid with an organic phase extraction solvent by using a multistage countercurrent extraction device, and extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent to obtain a loaded organic phase and a raffinate phase, wherein the loaded organic phase and the raffinate phase are extracted by the mixed acid;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that the mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain a mixed dilute acid solution;
step four, concentration: carrying out reduced pressure evaporation concentration on the mixed dilute acid solution through a reduced pressure evaporator to obtain mixed acid solution;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the ratio of the sulfuric acid to the phosphoric acid back to the usable range of the polishing solution by supplementing the sulfuric acid and the phosphoric acid.
As a further scheme of the invention: the organic phase extraction solvent is tributyl phosphate, kerosene or a mixture of tributyl phosphate and diisopropyl ether, wherein the volume ratio of the tributyl phosphate to the kerosene is 1:1-1:4, and the volume ratio of the tributyl phosphate to the diisopropyl ether is 1:0-2: 1.
As a further scheme of the invention: the extraction process adopts multi-stage countercurrent extraction, the extraction stage number is 4-8, the volume ratio of the organic phase extraction solvent to the chemical polishing waste liquid is 1:1-6:1, the single-stage extraction time is 5-30 minutes, and the stirring speed is 100-400 revolutions per minute.
As a further scheme of the invention: the back extraction process adopts multi-stage counter-current back extraction, the number of the back extraction stages is 4-8, the volume ratio of the loaded organic phase to the pure water is 1:1-1:6, the time of the single-stage back extraction is 5-30 minutes, and the stirring speed is 100-400 revolutions per minute.
As a further scheme of the invention: the pressure reduction evaporator is a corrosion-resistant low-temperature evaporator, steam is used as a heat source, the negative pressure is 0.02-0.09MPa, and the temperature is 65-85 ℃; the condensed water produced in the evaporation of the decompression evaporator is reused in the multistage countercurrent rinsing tank.
As a further scheme of the invention: the multistage countercurrent extraction device comprises a multistage countercurrent extraction mechanism and stirrers, wherein a plurality of stirrers are arranged on two sides of the top of the multistage countercurrent extraction mechanism in a penetrating mode, a heavy phase inlet and a light phase outlet are respectively arranged on two sides of the bottom of one end of the multistage countercurrent extraction mechanism, a heavy phase outlet and a light phase inlet are respectively arranged on two sides of the bottom of the other end of the multistage countercurrent extraction mechanism, the heavy phase inlet and the heavy phase outlet are located on the same side, and the light phase outlet and the light phase inlet are located on the same side.
As a further scheme of the invention: multistage countercurrent extraction mechanism comprises six extraction units, and adjacent extraction unit's installation opposite direction, the extraction unit includes the extraction box, set gradually mixing region, the district that stews, divide the liquid district in the inner chamber of extraction box, the (mixing) shaft of agitator is arranged in mixing region.
As a further scheme of the invention: an overflow plate and a guide plate are arranged at the joint of the mixing area and the standing area of the extraction box, the height of the overflow plate is lower than that of the guide plate, and a gap is arranged between the bottom of the guide plate and the bottom of an inner cavity of the extraction box; the extraction box is provided with a baffle at the junction of the standing area and the liquid separating area, and a liquid inlet is formed in one side of the bottom of the baffle.
As a further scheme of the invention: a support plate is vertically arranged in the middle of the bottom of the inner cavity of the mixing zone, a bottom plate is arranged at the top of the support plate, and a liquid inlet hole is formed in the axis of the bottom plate; two corners of one side of the inner cavity of the liquid separation area, which is far away from the baffle, are respectively provided with a light phase overflow inclined plate and a heavy phase limiting right-angle plate, the height of the light phase overflow inclined plate is lower than that of the heavy phase limiting right-angle plate, and a gap is arranged between the bottom of the heavy phase limiting right-angle plate and the bottom of the extraction box; and the mixing area and the liquid separating area of the adjacent extraction units are communicated.
As a further scheme of the invention: the working principle of the multistage countercurrent extraction device is as follows:
an organic phase extraction solvent enters a multistage countercurrent extraction mechanism from a light phase inlet, chemical polishing waste liquid enters the multistage countercurrent extraction mechanism from a heavy phase inlet, a stirrer is started, the stirrer operates to drive the organic phase extraction solvent and the chemical polishing waste liquid to be uniformly mixed in a mixing zone, the organic phase extraction solvent and the chemical polishing waste liquid are contacted in the multistage countercurrent extraction mechanism, mixed acid in the chemical polishing waste liquid is extracted into the organic phase extraction solvent, and a loaded organic phase and a raffinate phase are obtained after standing and layering in a standing zone;
the loaded organic phase is positioned on the upper layer of the raffinate phase, in the liquid separation zone, the raffinate phase flows to the mixing zone of the next extraction unit from the heavy phase inlet to the heavy phase outlet from a gap below the heavy phase limiting right-angle plate, and the loaded organic phase overflows from the upper part of the light phase overflow inclined plate to the mixing zone of the next extraction unit from the light phase inlet to the light phase outlet;
the closer the loaded organic phase is to the heavy phase inlet, the higher the content of the mixed acid in the raffinate phase is, so that more and more loaded organic phases are discharged from the light phase outlet after further extraction; the closer the raffinate phase is to the light phase inlet, the higher the content of the organic phase extraction solvent in the loaded organic phase is, so that after further extraction, the mixed acid content in the raffinate phase is less and less, and finally the raffinate phase is discharged to a sewage treatment system from the heavy phase outlet.
The invention has the beneficial effects that:
(1) the method for purifying and treating the chemical polishing waste liquid can fundamentally solve the problem of waste liquid treatment in the chemical polishing industry, and reduces the sewage treatment cost and the hazardous waste treatment cost of enterprises; the mode of the purification treatment of the chemical polishing waste liquid can control continuous operation, saves manpower, avoids the danger of concentrated acid manual operation, has small operation energy consumption, has an extraction rate of 80-85 percent, is beneficial to reducing the burden of enterprises, has higher environmental protection value, is beneficial to the development of enterprises, and is worthy of popularization;
(2) the invention relates to a mode for purifying and treating chemical polishing waste liquid, which comprises the steps of carrying out multistage countercurrent extraction by using a multistage countercurrent extraction device, enabling an organic phase extraction solvent to enter a multistage countercurrent extraction mechanism from a light phase inlet, enabling the chemical polishing waste liquid to enter the multistage countercurrent extraction mechanism from a heavy phase inlet, starting a stirrer, operating the stirrer to drive the organic phase extraction solvent and the chemical polishing waste liquid to be uniformly mixed in a mixing zone, enabling the organic phase extraction solvent and the chemical polishing waste liquid to be contacted in the multistage countercurrent extraction mechanism, extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent, and standing and layering in a standing zone to obtain a loaded organic phase and a raffinate phase; the loaded organic phase is positioned on the upper layer of the raffinate phase, in the liquid separation zone, the raffinate phase flows to the mixing zone of the next extraction unit from the heavy phase inlet to the heavy phase outlet from a gap below the heavy phase limiting right-angle plate, and the loaded organic phase overflows from the upper part of the light phase overflow inclined plate to the mixing zone of the next extraction unit from the light phase inlet to the light phase outlet; the closer the loaded organic phase is to the heavy phase inlet, the higher the content of the mixed acid in the raffinate phase is, so that more and more loaded organic phases are discharged from the light phase outlet after further extraction; the more the raffinate phase is close to the light phase inlet, the higher the content of the organic phase extraction solvent in the loaded organic phase is, so that after further extraction, the mixed acid content in the raffinate phase is less and less, and finally the raffinate phase is discharged to a sewage treatment system from the heavy phase outlet; this multistage countercurrent extraction device is through with organic phase extraction solvent, the chemical polishing waste liquid is with opposite direction input, make organic phase extraction solvent, countercurrent contact between the chemical polishing waste liquid, make the chemical polishing waste liquid from getting into multistage countercurrent extraction device to exhaust in-process, the content of the organic phase extraction solvent of contact is more and more, make remaining mixed acid fully extract to organic phase extraction solvent in the chemical polishing waste liquid, make the mixed acid content in the raffinate phase that the extraction chemical polishing waste liquid obtained low, the rate of recovery is high, the abundant that aluminium ion got rid of simultaneously, the purification treatment of chemical polishing waste liquid is effectual.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of one mode of the purification treatment of chemical polishing waste liquid in the present invention;
FIG. 2 is a schematic view of the structure of a multistage countercurrent extraction apparatus according to the present invention;
FIG. 3 is a schematic view of the internal structure of a multistage countercurrent extraction mechanism according to the present invention;
FIG. 4 is a schematic diagram of the structure of an extraction unit according to the present invention;
fig. 5 is a connection view of adjacent mixing and separating regions in the present invention.
In the figure: 10. a heavy phase inlet; 20. a heavy phase outlet; 30. a light phase outlet; 40. a light phase inlet; 101. a multi-stage counter-current extraction mechanism; 102. a stirrer; 103. a mixing zone; 104. a standing area; 105. a liquid separation zone; 106. an extraction box; 107. an overflow plate; 108. a baffle; 109. a baffle plate; 110. a liquid inlet; 111. a base plate; 112. a liquid inlet hole; 113. a support plate; 114. a light phase overflow sloping plate; 115. heavy phase limit right-angle plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
referring to fig. 1, the polishing solvent is a chemical polishing waste liquid containing sulfuric acid and phosphoric diacid, wherein the concentration of aluminum ions is 11g/L, the mass fraction of the mixed acid is 42%, and the density is 1.38 g/ml;
the embodiment is a method for purifying chemical polishing waste liquid, comprising the following steps:
step one, collection: mixing chemical polishing aging liquid in a chemical polishing tank with rinsing water from a multistage countercurrent rinsing tank, and filtering the mixture in a chemical polishing waste liquid collecting tank through a bag filter to obtain chemical polishing waste liquid;
step two, extraction: in an extraction tank, contacting the chemical polishing waste liquid with an organic phase extraction solvent by using a multistage countercurrent extraction device, extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent to obtain a loaded organic phase and an extraction raffinate phase, wherein the mixed acid is extracted, and the extraction raffinate phase enters a sewage treatment system;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that the mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain a mixed dilute acid solution;
step four, concentration: carrying out reduced pressure evaporation concentration on the mixed dilute acid solution through a reduced pressure evaporator to obtain a mixed acid solution and an eluted extraction solvent, and recycling the extraction solvent to the extraction process;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the ratio of the sulfuric acid to the phosphoric acid back to the usable range of the polishing solution by supplementing the sulfuric acid and the phosphoric acid.
The organic phase extraction solvent is a mixture of tributyl phosphate and kerosene, wherein the volume ratio of the tributyl phosphate to the kerosene is 1: 1.
The extraction process adopts multi-stage countercurrent extraction, the extraction stage number is 6, the volume ratio of the organic phase extraction solvent to the chemical polishing waste liquid is 4:1, the single-stage extraction time is 10 minutes, and the stirring speed is 260 revolutions per minute.
The back extraction process adopts multi-stage counter-current back extraction, the number of the back extraction stages is 4, the volume ratio of the loaded organic phase to the pure water is 1:3, the single-stage back extraction time is 12 minutes, and the stirring speed is 300 revolutions per minute.
The pressure reduction evaporator is a corrosion-resistant low-temperature evaporator, steam is used as a heat source, the negative pressure is 0.08MPa, and the temperature is not more than 80 ℃; the condensed water produced in the evaporation of the decompression evaporator is reused in the multistage countercurrent rinsing tank.
Wherein the mass fraction of the mixed acid in the raffinate phase obtained in the second step is 5%, and the concentration of aluminum ions is 22 g/L.
Wherein the concentration of aluminum ions in the mixed diluted acid obtained in the third step is 131 mg/L.
Wherein the density of the mixed acid liquid obtained in the fourth step is 1.62 g/ml.
Wherein the phosphorus-sulfur ratio measured in the fifth step is 7: 1.
Example 2:
referring to fig. 1, the polishing solvent is a chemical polishing waste liquid containing sulfuric acid and phosphoric diacid, wherein the concentration of aluminum ions is 13g/L, the mass fraction of the mixed acid is 45%, and the density is 1.42 g/ml;
the embodiment is a method for purifying chemical polishing waste liquid, comprising the following steps:
step one, collection: mixing chemical polishing aging liquid in a chemical polishing tank with rinsing water from a multistage countercurrent rinsing tank, and filtering the mixture in a chemical polishing waste liquid collecting tank through a bag filter to obtain chemical polishing waste liquid;
step two, extraction: in an extraction tank, contacting the chemical polishing waste liquid with an organic phase extraction solvent by using a multistage countercurrent extraction device, extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent to obtain a loaded organic phase and an extraction raffinate phase, wherein the mixed acid is extracted, and the extraction raffinate phase enters a sewage treatment system;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that the mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain a mixed dilute acid solution;
step four, concentration: carrying out reduced pressure evaporation concentration on the mixed dilute acid solution through a reduced pressure evaporator to obtain a mixed acid solution and an eluted extraction solvent, and recycling the extraction solvent to the extraction process;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the ratio of the sulfuric acid to the phosphoric acid back to the usable range of the polishing solution by supplementing the sulfuric acid and the phosphoric acid.
The organic phase extraction solvent is a mixture of tributyl phosphate and kerosene, wherein the volume ratio of the tributyl phosphate to the kerosene is 2: 1.
The extraction process adopts multi-stage countercurrent extraction, the extraction stage number is 6, the volume ratio of the organic phase extraction solvent to the chemical polishing waste liquid is 4:1, the single-stage extraction time is 10 minutes, and the stirring speed is 300 revolutions per minute.
The back extraction process adopts multi-stage counter-current back extraction, the number of the back extraction stages is 4, the volume ratio of the loaded organic phase to the pure water is 1:3, the single-stage back extraction time is 8 minutes, and the stirring speed is 200 revolutions per minute.
The pressure reduction evaporator is a corrosion-resistant low-temperature evaporator, steam is used as a heat source, the negative pressure is 0.07MPa, and the temperature is not more than 80 ℃; the condensed water produced in the evaporation of the decompression evaporator is reused in the multistage countercurrent rinsing tank.
Wherein the mass fraction of the mixed acid in the raffinate phase obtained in the second step is 6%, and the concentration of aluminum ions is 25 g/L.
Wherein the concentration of aluminum ions in the mixed diluted acid obtained in the third step is 116 mg/L.
Wherein the density of the mixed acid liquid obtained in the fourth step is 1.67 g/ml.
Wherein the phosphorus-sulfur ratio measured in the fifth step is 7.3: 1.
Example 3:
referring to fig. 2-5, the multistage countercurrent extraction apparatus in this embodiment includes a multistage countercurrent extraction mechanism 101 and stirrers 102, wherein a plurality of stirrers 102 are installed through both sides of the top of the multistage countercurrent extraction mechanism 101, a heavy phase inlet 10 and a light phase outlet 30 are respectively installed on both sides of the bottom of one end of the multistage countercurrent extraction mechanism 101, a heavy phase outlet 20 and a light phase inlet 40 are respectively installed on both sides of the bottom of the other end of the multistage countercurrent extraction mechanism 101, the heavy phase inlet 10 and the heavy phase outlet 20 are located on the same side, and the light phase outlet 30 and the light phase inlet 40 are located on the same side;
the multistage countercurrent extraction mechanism 101 is composed of six extraction units, the installation directions of adjacent extraction units are opposite, each extraction unit comprises an extraction box 106, a mixing area 103, a standing area 104 and a liquid separation area 105 are sequentially arranged in the inner cavity of each extraction box 106, and a stirring shaft of the stirrer 102 is positioned in the mixing area 103;
an overflow plate 107 and a guide plate 108 are arranged at the joint of the mixing area 103 and the standing area 104 of the extraction tank 106, the height of the overflow plate 107 is lower than that of the guide plate 108, and a gap is arranged between the bottom of the guide plate 108 and the bottom of an inner cavity of the extraction tank 106; a baffle 109 is arranged at the joint of the standing area 104 and the liquid separating area 105 of the extraction box 106, and a liquid inlet 110 is formed in one side of the bottom of the baffle 109;
a support plate 113 is vertically arranged in the middle of the bottom of the inner cavity of the mixing zone 103, a bottom plate 111 is arranged at the top of the support plate 113, and a liquid inlet hole 112 is formed in the axis of the bottom plate 111; two corners of the inner cavity of the liquid separation zone 105, which are far away from the baffle 109, are respectively provided with a light phase overflow inclined plate 114 and a heavy phase limit right-angle plate 115, the height of the light phase overflow inclined plate 114 is lower than that of the heavy phase limit right-angle plate 115, and a gap is formed between the bottom of the heavy phase limit right-angle plate 115 and the bottom of the extraction box 106; the mixing zone 103 and the separating zone 105 of the adjacent extraction units are in communication.
Referring to fig. 1-5, the multi-stage countercurrent extraction apparatus of the present embodiment operates as follows:
an organic phase extraction solvent enters a multistage countercurrent extraction mechanism 101 from a light phase inlet 40, a chemical polishing waste liquid enters the multistage countercurrent extraction mechanism 101 from a heavy phase inlet 10, a stirrer 102 is started, the stirrer 102 operates to drive the organic phase extraction solvent and the chemical polishing waste liquid to be uniformly mixed in a mixing zone 103, the organic phase extraction solvent and the chemical polishing waste liquid are contacted in the multistage countercurrent extraction mechanism 101, mixed acid in the chemical polishing waste liquid is extracted into the organic phase extraction solvent, and a loaded organic phase and a raffinate phase are obtained after standing and layering in a standing zone 104;
the loaded organic phase is positioned at the upper layer of the raffinate phase, in the liquid separation zone 105, the raffinate phase flows to the mixing zone 103 of the next extraction unit from the heavy phase inlet 10 to the heavy phase outlet 20 from the gap below the heavy phase limiting right-angle plate 115, and the loaded organic phase overflows from the upper part of the light phase overflow inclined plate 114 to the mixing zone 103 of the next extraction unit from the light phase inlet 40 to the light phase outlet 30;
the closer the loaded organic phase is to the heavy phase inlet 10, the higher the content of the mixed acid in the raffinate phase contacted with the loaded organic phase is, so that after further extraction, more and more loaded organic phases are discharged from the light phase outlet 30; the closer the raffinate phase is to the light phase inlet 40, the higher the content of the organic phase extraction solvent in the loaded organic phase is, so that after further extraction, the mixed acid content in the raffinate phase becomes smaller and smaller, and finally the raffinate phase is discharged from the heavy phase outlet 20 to a sewage treatment system.
This multistage countercurrent extraction device is through with organic phase extraction solvent, the chemical polishing waste liquid is with opposite direction input, make organic phase extraction solvent, countercurrent contact between the chemical polishing waste liquid, make the chemical polishing waste liquid from getting into multistage countercurrent extraction device to exhaust in-process, the content of the organic phase extraction solvent of contact is more and more, make remaining mixed acid fully extract to organic phase extraction solvent in the chemical polishing waste liquid, make the mixed acid content in the raffinate phase that the extraction chemical polishing waste liquid obtained low, the rate of recovery is high, the abundant that aluminium ion got rid of simultaneously, the purification treatment of chemical polishing waste liquid is effectual.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (9)
1. A method for purifying chemical polishing waste liquid is characterized by comprising the following steps:
step one, collection: mixing chemical polishing aging liquid in a chemical polishing tank with rinsing water from a multistage countercurrent rinsing tank, and filtering the mixture in a chemical polishing waste liquid collecting tank through a bag filter to obtain chemical polishing waste liquid;
step two, extraction: in an extraction tank, contacting the chemical polishing waste liquid with an organic phase extraction solvent by using a multistage countercurrent extraction device, and extracting mixed acid in the chemical polishing waste liquid into the organic phase extraction solvent to obtain a loaded organic phase and a raffinate phase, wherein the loaded organic phase and the raffinate phase are extracted by the mixed acid;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that the mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain a mixed dilute acid solution;
step four, concentration: carrying out reduced pressure evaporation concentration on the mixed dilute acid solution through a reduced pressure evaporator to obtain mixed acid solution;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the ratio of the sulfuric acid to the phosphoric acid back to the usable range of the polishing solution by supplementing the sulfuric acid and the phosphoric acid.
2. The method according to claim 1, wherein the organic phase extraction solvent is tributyl phosphate, kerosene or a mixture of tributyl phosphate and diisopropyl ether, wherein the volume ratio of tributyl phosphate to kerosene is 1:1-1:4, and the volume ratio of tributyl phosphate to diisopropyl ether is 1:0-2: 1.
3. The method as claimed in claim 1, wherein the extraction process comprises a multi-stage countercurrent extraction process, the number of extraction stages is 4-8, the volume ratio of the organic phase extraction solvent to the chemical polishing waste liquid is 1:1-6:1, the single-stage extraction time is 5-30 min, and the stirring speed is 100-400 rpm.
4. The method as claimed in claim 1, wherein the back-extraction process comprises a multi-stage counter-current back-extraction, the number of the back-extraction stages is 4-8, the volume ratio of the loaded organic phase to the pure water is 1:1-1:6, the time of the single-stage back-extraction is 5-30 min, and the stirring speed is 100-400 rpm.
5. The method according to claim 1, wherein the reduced-pressure evaporator is a corrosion-resistant low-temperature evaporator, steam is used as a heat source, the negative pressure is 0.02-0.09MPa, and the temperature is 65-85 ℃; the condensed water produced in the evaporation of the decompression evaporator is reused in the multistage countercurrent rinsing tank.
6. The method of claim 1, wherein the multistage countercurrent extraction apparatus comprises a multistage countercurrent extraction mechanism (101) and a plurality of stirrers (102), wherein a plurality of stirrers (102) are installed on two sides of the top of the multistage countercurrent extraction mechanism (101), a heavy phase inlet (10) and a light phase outlet (30) are respectively arranged on two sides of the bottom of one end of the multistage countercurrent extraction mechanism (101), a heavy phase outlet (20) and a light phase inlet (40) are respectively arranged on two sides of the bottom of the other end of the multistage countercurrent extraction mechanism (101), the heavy phase inlet (10) and the heavy phase outlet (20) are located on the same side, and the light phase outlet (30) and the light phase inlet (40) are located on the same side.
7. A chemical polishing waste liquid purification treatment mode according to claim 6, characterized in that the multistage countercurrent extraction mechanism (101) is composed of six extraction units, the installation directions of adjacent extraction units are opposite, the extraction units comprise extraction boxes (106), a mixing zone (103), a standing zone (104) and a liquid separation zone (105) are sequentially arranged in the inner cavity of the extraction box (106), and the stirring shaft of the stirrer (102) is positioned in the mixing zone (103).
8. The method of claim 7, wherein the extraction tank (106) is provided with an overflow plate (107) and a flow guide plate (108) at the joint of the mixing zone (103) and the standing zone (104), the height of the overflow plate (107) is lower than that of the flow guide plate (108), and a gap is arranged between the bottom of the flow guide plate (108) and the bottom of the inner cavity of the extraction tank (106); a baffle (109) is arranged at the joint of the standing area (104) and the liquid distribution area (105) of the extraction box (106), and a liquid inlet (110) is formed in one side of the bottom of the baffle (109).
9. The method for purifying chemical polishing waste liquid according to claim 8, wherein a support plate (113) is vertically arranged at the middle position of the bottom of the inner cavity of the mixing zone (103), a bottom plate (111) is installed at the top of the support plate (113), and a liquid inlet hole (112) is formed at the axis of the bottom plate (111); two corners of one side of an inner cavity of the liquid distribution area (105) far away from the baffle (109) are respectively provided with a light phase overflow inclined plate (114) and a heavy phase limiting right-angle plate (115), the height of the light phase overflow inclined plate (114) is lower than that of the heavy phase limiting right-angle plate (115), and a gap is formed between the bottom of the heavy phase limiting right-angle plate (115) and the bottom of the extraction box (106); the mixing area (103) and the liquid separation area (105) of the adjacent extraction units are communicated.
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