CN112299635B - Method for purifying chemical polishing waste liquid - Google Patents
Method for purifying chemical polishing waste liquid Download PDFInfo
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- CN112299635B CN112299635B CN202011139595.0A CN202011139595A CN112299635B CN 112299635 B CN112299635 B CN 112299635B CN 202011139595 A CN202011139595 A CN 202011139595A CN 112299635 B CN112299635 B CN 112299635B
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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
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- 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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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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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 chemical polishing industry, reduces the sewage treatment cost and the hazardous waste treatment cost of enterprises, and has the advantages that the recovery mode of mixed acid in chemical polishing waste liquid is unique, the extraction mode and equipment are selected, the selected extraction solvent can be recycled, the service life of the equipment is long, the purchasing cost of enterprises can be reduced, and no new waste liquid or sludge is generated in the chemical polishing waste liquid treatment process by adopting closed-loop operation, so that the method is a complete green recycling process; the method for purifying the chemical polishing waste liquid can control continuous operation, saves labor, avoids the danger of manually operating concentrated acid, has low operation energy consumption, has extraction rate of 80-85%, is favorable for lightening the burden of enterprises, has higher environmental protection value, is favorable for the development of enterprises, 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 leveling etching by means of the selective dissolution of the uneven areas on the surface of a sample by chemical etching of chemical reagents. The polishing solution has the advantages of simple equipment, capability of processing thin pipes, parts with deep holes and complex shapes, production efficiency improvement, and one of the disadvantages is short service life of the polishing solution and difficult adjustment and regeneration of the solution concentration.
The typical chemical polishing solutions are diacid or triacid solutions, the general composition of which is: 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 general components: 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, due to continuous dissolution of metal parts, hydrogen ion consumption and continuous increase of metal ion concentrations of aluminum, iron and the like, the polishing effect of the polishing solution is gradually deteriorated, and the polishing solution is called chemical polishing aging liquid. The common treatment mode of the chemical polishing aging liquid is to discharge a part of the chemical polishing aging liquid and supplement new acid according to a proportion so as to ensure that the chemical polishing tank liquid meets the process requirements. The discharged chemical polishing 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 surface of the metal part after chemical polishing can also carry part of the polishing solution, so the rinsing water can 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 lack of an effective recycling method for the chemical polishing waste liquid has higher cost when being treated by a qualified hazardous waste treatment unit, and if the chemical polishing waste liquid is treated as waste water in a sewage station, a large amount of alkali is consumed, a large amount of sludge is generated, so that the cost of the medicament is high, and the cost waste of acid liquor is caused.
The existing disposal mode of chemical throwing waste liquid faces the problems of low recovery rate or higher equipment investment and operation cost, so that the development of a purification mode capable of effectively recycling valuable components in the waste liquid and reducing comprehensive cost is a key of the invention.
Disclosure of Invention
In order to overcome the technical problems described above, the present invention aims to provide a method for purifying chemical polishing waste liquid: the method 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 chemical polishing waste liquid to enter the multistage countercurrent extraction mechanism from a heavy phase inlet, starting a stirrer, driving 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 contact 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, and in the liquid separation zone, the raffinate phase flows from a gap below the heavy phase limiting rectangular plate to a mixing zone of a next extraction unit from the heavy phase inlet to the heavy phase outlet, and overflows from the upper part of the light phase overflow inclined plate to a 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 mixed acid in the raffinate phase is, so that after further extraction, the loaded organic phase is more and more, and finally the mixed acid is discharged from the light phase outlet; the organic phase extraction solvent content in the loaded organic phase contacted with the light phase inlet is higher as the raffinate phase is closer to the light phase inlet, so that the content of mixed acid in the raffinate phase is smaller after further extraction, and finally the mixed acid is discharged to a sewage treatment system from the heavy phase outlet, thereby solving the problems of low recovery rate or higher equipment investment and operation cost of the existing chemical polishing waste liquid treatment mode.
The aim of the invention can be achieved by the following technical scheme:
a method for purifying chemical polishing waste liquid comprises the following steps:
step one, collecting: combining chemical polishing aging liquid in the chemical polishing tank with rinsing water from the multi-stage countercurrent rinsing tank, and filtering the chemical polishing aging liquid 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 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 from which the mixed acid is extracted;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain mixed dilute acid solution;
step four, concentrating: the mixed dilute acid solution is subjected to reduced pressure evaporation concentration 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 proportion of sulfuric acid and phosphoric acid to adjust the usable range of the chemical polishing liquid by supplementing sulfuric acid and 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 tributyl phosphate to kerosene is 1:1-1:4, and the volume ratio of tributyl phosphate to diisopropyl ether is 1:0-2:1.
As a further scheme of the invention: the extraction process adopts multistage 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 rotation speed is 100-400 rpm.
As a further scheme of the invention: the back extraction process adopts multistage countercurrent back extraction, the back extraction stage number is 4-8, the volume ratio of the loaded organic phase to the pure water is 1:1-1:6, the single-stage back extraction time is 5-30 minutes, and the stirring rotating speed is 100-400 rpm.
As a further scheme of the invention: the decompression 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 ℃; condensed water generated during evaporation of the decompression evaporator is recycled to the multi-stage 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 installed 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: the multistage countercurrent extraction mechanism consists of six extraction units, the installation directions of the adjacent extraction units are opposite, the extraction units comprise extraction boxes, a mixing area, a standing area and a liquid separation area are sequentially arranged in the inner cavities of the extraction boxes, and the stirring shaft of the stirrer is positioned in the mixing area.
As a further scheme of the invention: the extraction box is provided with an overflow plate and a guide plate at the joint of the mixing area and the standing area, 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 the inner cavity of the extraction box; the extraction box is provided with a baffle at the joint of the standing area and the liquid dividing area, and a liquid inlet is formed in one side of the bottom of the baffle.
As a further scheme of the invention: a supporting 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 supporting plate, and a liquid inlet is formed in the axis of the bottom plate; a light-phase overflow inclined plate and a heavy-phase limit rectangular plate are respectively arranged at two corners of one side, far away from the baffle, of the inner cavity of the liquid separation zone, the height of the light-phase overflow inclined plate is lower than that of the heavy-phase limit rectangular plate, and a gap is formed between the bottom of the heavy-phase limit rectangular plate and the bottom of the extraction box; the mixing areas and the liquid dividing areas 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:
the organic phase extraction solvent enters a multistage countercurrent extraction mechanism from a light phase inlet, the chemical polishing waste liquid enters the multistage countercurrent extraction mechanism from a heavy phase inlet, a stirrer is started, the stirrer is operated 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 load 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, and in the liquid separation zone, the raffinate phase flows from a gap below the heavy phase limiting rectangular plate to a mixing zone of a next extraction unit from the heavy phase inlet to the heavy phase outlet, and overflows from the upper part of the light phase overflow inclined plate to a 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 mixed acid in the raffinate phase is, so that after further extraction, the loaded organic phase is more and more, and finally the mixed acid is discharged from the light phase outlet; the nearer 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 content of mixed acid in the raffinate phase is smaller and smaller, and finally the mixed acid is discharged to a sewage treatment system from a heavy phase outlet.
The invention has the beneficial effects that:
(1) The method for purifying the chemical polishing waste liquid can fundamentally solve the problem of waste liquid treatment in the chemical polishing industry, reduces the sewage treatment cost and the hazardous waste treatment cost of enterprises, adopts a unique recovery mode of mixed acid in chemical polishing waste liquid, adopts an extraction mode and equipment, and adopts a recyclable extraction solvent, has long service life, can reduce the purchasing cost of enterprises, does not generate any new waste liquid and sludge in the chemical polishing waste liquid treatment process by adopting closed-loop operation, and is a complete green recycling process; the method for purifying the chemical polishing waste liquid can control continuous operation, saves labor, avoids the danger of manually operating concentrated acid, has low operation energy consumption, has the extraction rate of 80-85%, is beneficial to reducing the burden of enterprises, has higher environmental protection value, is beneficial to the development of the enterprises, and is worthy of popularization;
(2) According to the method for purifying the chemical polishing waste liquid, a multistage countercurrent extraction device is used for multistage countercurrent extraction, organic phase extraction solvent enters a multistage countercurrent extraction mechanism from a light phase inlet, the chemical polishing waste liquid enters the multistage countercurrent extraction mechanism from a heavy phase inlet, a stirrer is started, the stirrer is operated 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 after standing and layering in a standing zone, a loaded organic phase and a raffinate phase are obtained; the loaded organic phase is positioned on the upper layer of the raffinate phase, and in the liquid separation zone, the raffinate phase flows from a gap below the heavy phase limiting rectangular plate to a mixing zone of a next extraction unit from the heavy phase inlet to the heavy phase outlet, and overflows from the upper part of the light phase overflow inclined plate to a 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 mixed acid in the raffinate phase is, so that after further extraction, the loaded organic phase is more and more, and finally the mixed acid is discharged from the light phase outlet; the organic phase extraction solvent content in the loaded organic phase contacted with the light phase inlet is higher as the raffinate phase is closer to the light phase inlet, so that the mixed acid content in the raffinate phase is smaller after further extraction, and finally the mixed acid is discharged to a sewage treatment system from the heavy phase outlet; according to the multistage countercurrent extraction device, the organic phase extraction solvent and the chemical polishing waste liquid are input in opposite directions, so that the organic phase extraction solvent and the chemical polishing waste liquid are in countercurrent contact, the content of the contacted organic phase extraction solvent is increased from entering the multistage countercurrent extraction device to being discharged, residual mixed acid in the chemical polishing waste liquid is fully extracted to the organic phase extraction solvent, the content of the mixed acid in a raffinate phase obtained by extracting the chemical polishing waste liquid is low, the recovery rate is high, meanwhile, aluminum ions are fully removed, and the purification treatment effect of the chemical polishing waste liquid is good.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of one manner of purifying a chemical polishing waste liquid in accordance with the present invention;
FIG. 2 is a schematic diagram of a multistage countercurrent extraction apparatus according to the present invention;
FIG. 3 is a schematic diagram of the internal structure of the multistage countercurrent extraction mechanism of the present invention;
FIG. 4 is a schematic diagram of the structure of the extraction unit of the present invention;
FIG. 5 is a view showing the connection of adjacent mixing and dividing zones 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 multistage countercurrent extraction mechanism; 102. a stirrer; 103. a mixing zone; 104. a standing area; 105. a liquid separation area; 106. an extraction box; 107. an overflow plate; 108. a deflector; 109. a baffle; 110. a liquid inlet; 111. a bottom plate; 112. a liquid inlet hole; 113. a support plate; 114. a light phase overflow sloping plate; 115. and a heavy phase limiting right angle plate.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
referring to FIG. 1, the treatment polishing solvent is chemical polishing waste liquid containing sulfuric acid and phosphoric acid diacid, wherein the concentration of aluminum ions is 11g/L, the mass fraction of the concentration of mixed acid is 42%, and the density is 1.38g/ml;
the embodiment is a method for purifying chemical polishing waste liquid, comprising the following steps:
step one, collecting: combining chemical polishing aging liquid in the chemical polishing tank with rinsing water from the multi-stage countercurrent rinsing tank, and filtering the chemical polishing aging liquid 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, a multistage countercurrent extraction device is used for contacting chemical polishing waste liquid with an organic phase extraction solvent, mixed acid in the chemical polishing waste liquid is extracted into the organic phase extraction solvent, a loaded organic phase and a raffinate phase of the extracted mixed acid are obtained, and the 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 mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain mixed dilute acid solution;
step four, concentrating: the mixed dilute acid solution is subjected to reduced pressure evaporation concentration through a reduced pressure evaporator to obtain mixed acid solution and eluted extraction solvent, and the extraction solvent is recycled to the extraction process;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the proportion of sulfuric acid and phosphoric acid to adjust the usable range of the chemical polishing liquid by supplementing sulfuric acid and 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 multistage 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 rotation speed is 260 revolutions per minute.
The back extraction process adopts multistage countercurrent back extraction, the back extraction stage number 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 rotation speed is 300 revolutions per minute.
The decompression 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 ℃; condensed water generated during evaporation of the decompression evaporator is recycled to the multi-stage countercurrent rinsing tank.
Wherein the mass fraction of the concentration of the mixed acid in the raffinate phase obtained in the second step is 5%, and the concentration of aluminum ions is 22g/L.
Wherein the concentration of aluminum ions in the mixed dilute acid obtained in the step three is 131mg/L.
Wherein the density of the mixed acid liquid obtained in the step four is 1.62g/ml.
Wherein the phosphorus-sulfur ratio measured in the fifth step is 7:1.
Example 2:
referring to FIG. 1, the treatment polishing solvent is chemical polishing waste liquid containing sulfuric acid and phosphoric acid diacid, wherein the concentration of aluminum ions is 13g/L, the mass fraction of the concentration of mixed acid is 45%, and the density is 1.42g/ml;
the embodiment is a method for purifying chemical polishing waste liquid, comprising the following steps:
step one, collecting: combining chemical polishing aging liquid in the chemical polishing tank with rinsing water from the multi-stage countercurrent rinsing tank, and filtering the chemical polishing aging liquid 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, a multistage countercurrent extraction device is used for contacting chemical polishing waste liquid with an organic phase extraction solvent, mixed acid in the chemical polishing waste liquid is extracted into the organic phase extraction solvent, a loaded organic phase and a raffinate phase of the extracted mixed acid are obtained, and the 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 mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain mixed dilute acid solution;
step four, concentrating: the mixed dilute acid solution is subjected to reduced pressure evaporation concentration through a reduced pressure evaporator to obtain mixed acid solution and eluted extraction solvent, and the extraction solvent is recycled to the extraction process;
and fifthly, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the proportion of sulfuric acid and phosphoric acid to adjust the usable range of the chemical polishing liquid by supplementing sulfuric acid and 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 multistage 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 rotation speed is 300 revolutions per minute.
The back extraction process adopts multistage countercurrent back extraction, the back extraction stage number 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 rotation speed is 200 rpm.
The decompression 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 ℃; condensed water generated during evaporation of the decompression evaporator is recycled to the multi-stage countercurrent rinsing tank.
Wherein the mass fraction of the concentration of the mixed acid in the raffinate phase obtained in the second step is 6%, and the concentration of the aluminum ions is 25g/L.
Wherein the concentration of aluminum ions in the mixed dilute acid obtained in the step three is 116mg/L.
Wherein the density of the mixed acid liquid obtained in the step four is 1.67g/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 device in this embodiment includes a multistage countercurrent extraction mechanism 101 and agitators 102, wherein a plurality of agitators 102 are installed on two sides of the top of the multistage countercurrent extraction mechanism 101 in a penetrating manner, a heavy phase inlet 10 and a light phase outlet 30 are respectively provided 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 provided 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;
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 an extraction box 106, a mixing region 103, a standing region 104 and a liquid separation region 105 are sequentially arranged in the inner cavity of the extraction box 106, and a stirring shaft of the stirrer 102 is positioned in the mixing region 103;
the extraction box 106 is provided with an overflow plate 107 and a guide plate 108 at the joint of the mixing area 103 and the standing area 104, 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 the inner cavity of the extraction box 106; the extraction box 106 is provided with a baffle 109 at the joint of the standing area 104 and the liquid separation area 105, and a liquid inlet 110 is arranged at one side of the bottom of the baffle 109;
a supporting 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 supporting plate 113, and a liquid inlet 112 is formed in the axis of the bottom plate 111; a light-phase overflow inclined plate 114 and a heavy-phase limit rectangular plate 115 are respectively arranged at two corners of one side of the inner cavity of the liquid separation zone 105, which is far away from the baffle 109, the height of the light-phase overflow inclined plate 114 is lower than that of the heavy-phase limit rectangular plate 115, and a gap is arranged between the bottom of the heavy-phase limit rectangular plate 115 and the bottom of the extraction box 106; the mixing zone 103 and the liquid separation zone 105 of the adjacent extraction units are in communication.
Referring to fig. 1 to 5, the multistage countercurrent extraction device in this embodiment works as follows:
the organic phase extraction solvent enters the multistage countercurrent extraction mechanism 101 from the light phase inlet 40, the chemical polishing waste liquid enters the multistage countercurrent extraction mechanism 101 from the heavy phase inlet 10, the stirrer 102 is started, the stirrer 102 is operated to drive the organic phase extraction solvent and the chemical polishing waste liquid to be uniformly mixed in the mixing zone 103, the organic phase extraction solvent and the chemical polishing waste liquid are contacted in the multistage countercurrent extraction mechanism 101, the mixed acid in the chemical polishing waste liquid is extracted into the organic phase extraction solvent, and the organic phase and the raffinate phase are obtained after the mixture is kept stand and layered in the standing zone 104;
the loaded organic phase is located at the upper layer of the raffinate phase, and in the liquid separation zone 105, the raffinate phase flows from a gap below the heavy phase limiting rectangular plate 115 to the mixing zone 103 of the next extraction unit from the heavy phase inlet 10 to the heavy phase outlet 20, 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 mixed acid content in the contact raffinate phase, so that after further extraction, the more the loaded organic phase is, and finally discharged from the light phase outlet 30; the closer the raffinate phase is to the light phase inlet 40, the higher the organic phase extraction solvent content in the loaded organic phase is, so that after further extraction, the less mixed acid content in the raffinate phase is, and finally discharged from the heavy phase outlet 20 to a sewage treatment system.
According to the multistage countercurrent extraction device, the organic phase extraction solvent and the chemical polishing waste liquid are input in opposite directions, so that the organic phase extraction solvent and the chemical polishing waste liquid are in countercurrent contact, the content of the contacted organic phase extraction solvent is increased from entering the multistage countercurrent extraction device to being discharged, residual mixed acid in the chemical polishing waste liquid is fully extracted to the organic phase extraction solvent, the content of the mixed acid in a raffinate phase obtained by extracting the chemical polishing waste liquid is low, the recovery rate is high, meanwhile, aluminum ions are fully removed, and the purification treatment effect of the chemical polishing waste liquid is good.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, 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 present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. 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 merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (1)
1. A method for purifying chemical polishing waste liquid, comprising the steps of:
step one, collecting: combining chemical polishing aging liquid in the chemical polishing tank with rinsing water from the multi-stage countercurrent rinsing tank, and filtering the chemical polishing aging liquid 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 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 from which the mixed acid is extracted;
step three, back extraction: in a back extraction tank, the loaded organic phase is contacted with pure water for back extraction, so that mixed acid is back extracted from the loaded organic phase and then enters the pure water to obtain mixed dilute acid solution;
step four, concentrating: the mixed dilute acid solution is subjected to reduced pressure evaporation concentration through a reduced pressure evaporator to obtain mixed acid solution;
step five, detecting the phosphorus-sulfur ratio of the mixed acid liquid, and adjusting the proportion of sulfuric acid and phosphoric acid to adjust the usable range of the chemical polishing liquid by supplementing sulfuric acid and phosphoric acid;
the multistage countercurrent extraction device comprises a multistage countercurrent extraction mechanism (101) and stirrers (102), wherein a plurality of stirrers (102) are installed on two sides of the top of the multistage countercurrent extraction mechanism (101) in a penetrating manner, 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 positioned on the same side, and the light phase outlet (30) and the light phase inlet (40) are positioned 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, the extraction units comprise extraction boxes (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);
the extraction box (106) is provided with an overflow plate (107) and a 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 guide plate (108), and a gap is arranged between the bottom of the guide plate (108) and the bottom of the inner cavity of the extraction box (106); the extraction box (106) is provided with a baffle (109) at the joint of the standing area (104) and the liquid dividing area (105), and a liquid inlet (110) is formed in one side of the bottom of the baffle (109);
a supporting 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 supporting plate (113), and a liquid inlet hole (112) is formed in the axis of the bottom plate (111); a light-phase overflow inclined plate (114) and a heavy-phase limit rectangular plate (115) are respectively arranged at two corners of one side, far away from the baffle plate (109), of the inner cavity of the liquid separation zone (105), the height of the light-phase overflow inclined plate (114) is lower than that of the heavy-phase limit rectangular plate (115), and a gap is formed between the bottom of the heavy-phase limit rectangular plate (115) and the bottom of the extraction box (106); the mixing zone (103) and the liquid dividing zone (105) of the adjacent extraction units are communicated;
the organic phase extraction solvent enters a multistage countercurrent extraction mechanism (101) from a light phase inlet (40), the 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 load 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, and flows from a gap below the heavy phase limiting rectangular plate (115) to a mixing zone (103) of the next extraction unit from the heavy phase inlet (10) to the heavy phase outlet (20) in the liquid separation zone (105), and 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 mixed acid in the raffinate phase contacted with the heavy phase inlet (10) is, so that after further extraction, the loaded organic phase is more and more, and finally the mixed acid is discharged from the light phase outlet (30);
the nearer the raffinate phase is to the light phase inlet (40), the higher the content of organic phase extraction solvent in the loaded organic phase is, so that after further extraction, the content of mixed acid in the raffinate phase is smaller and smaller, and finally the mixed acid is discharged to a sewage treatment system from the heavy phase outlet (20);
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;
the extraction process adopts multistage countercurrent extraction, 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 rotation speed is 100-400 rpm;
the back extraction process adopts multistage countercurrent back extraction, the back extraction stage number is 4-8, the volume ratio of the loaded organic phase to the pure water is 1:1-1:6, the single-stage back extraction time is 5-30 minutes, and the stirring rotating speed is 100-400 rpm;
the decompression 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 ℃; condensed water generated during evaporation of the decompression evaporator is recycled to the multi-stage countercurrent rinsing tank.
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