CN115536221B - Method for purifying heavy metal sludge - Google Patents
Method for purifying heavy metal sludge Download PDFInfo
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- CN115536221B CN115536221B CN202110715528.7A CN202110715528A CN115536221B CN 115536221 B CN115536221 B CN 115536221B CN 202110715528 A CN202110715528 A CN 202110715528A CN 115536221 B CN115536221 B CN 115536221B
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- metal sludge
- purifying
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- 239000010802 sludge Substances 0.000 title claims abstract description 150
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000003756 stirring Methods 0.000 claims abstract description 121
- 239000012629 purifying agent Substances 0.000 claims abstract description 40
- 238000002161 passivation Methods 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 99
- 229910021536 Zeolite Inorganic materials 0.000 claims description 48
- 239000010457 zeolite Substances 0.000 claims description 48
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 24
- 238000000746 purification Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 18
- 239000012690 zeolite precursor Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000000292 calcium oxide Substances 0.000 claims description 16
- 235000012255 calcium oxide Nutrition 0.000 claims description 16
- 239000003814 drug Substances 0.000 claims description 16
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 15
- 238000002791 soaking Methods 0.000 claims description 15
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 13
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 12
- 239000001110 calcium chloride Substances 0.000 claims description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 12
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 12
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 8
- 229910052680 mordenite Inorganic materials 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 230000001502 supplementing effect Effects 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 21
- 239000003795 chemical substances by application Substances 0.000 abstract description 8
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 8
- 239000003344 environmental pollutant Substances 0.000 abstract description 4
- 231100000719 pollutant Toxicity 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000005661 hydrophobic surface Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 241000605222 Acidithiobacillus ferrooxidans Species 0.000 description 1
- 241000605272 Acidithiobacillus thiooxidans Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000010668 complexation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a method for purifying heavy metal sludge, which comprises the following steps: 1) Collecting heavy metal sludge through a sludge collecting tank; 2) Conveying heavy metal sludge and a purifying agent into a stirring mixer through a first slurry pump, and stirring and uniformly mixing for 5-24 hours, wherein the stirring mixer adopts a positive rotation and reverse rotation alternating mode for stirring; 3) And (3) conveying the heavy metal sludge after uniform stirring and mixing into a passivation pool, maintaining the temperature at 35-60 ℃ and the water content at 30-60%, and carrying out passivation treatment for 120-200 hours. The method for purifying the heavy metal sludge is simple to operate and low in cost, can efficiently purify heavy metal pollutants and organic pollutants in the sludge, can realize recycling of the sludge, and utilizes environmental protection; the invention can realize the multiple stirring and mixing of the purifying agent and the sludge, thereby improving the mixing effect of the agent and the sludge and finally improving the purifying effect of the sludge.
Description
Technical Field
The invention relates to the technical field of sludge treatment, in particular to a method for purifying heavy metal sludge.
Background
Urban sewage treatment plants can produce a large amount of sludge, which contains a large amount of heavy metal pollutants and also contains part of organic pollutants. Heavy metals have the characteristics of difficult migration, easy enrichment, large harm and the like, so that the sludge can be discharged or recycled after purification treatment. The current common treatment method of heavy metal sludge comprises the following steps:
(1) Adsorption method
Separating and removing heavy metals by utilizing substances with special structures or chemical components;
(2) Chemical leaching method
Reducing the acidity of the sludge by sulfuric acid, hydrochloric acid or nitric acid and the like, and forming soluble metal ions by dissolving indissolvable metal compounds;
(3) Electric repair method
The electric technology is initially applied to the removal of soil heavy metals in the 80 th century, and the application in the removal of municipal sludge heavy metals is just started;
(4) Biological leaching method
Bioleaching is a technology which utilizes microorganisms in nature to produce oxidation, reduction, complexation or dissolution by direct action or indirect action of other metabolites, and separates and extracts certain insoluble components such as heavy metals in a solid phase, wherein the most widely used technologies are thiobacillus ferrooxidans and thiobacillus thiooxidans.
The adsorption method has the characteristics of simple treatment, low cost and the like, and has good application prospect. However, the adsorption method commonly adopted at present has the defect that the purification effect cannot meet the requirement, and limits the popularization and application of the adsorption method.
There is a need to provide a more reliable solution.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for purifying heavy metal sludge aiming at the defects in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for purifying heavy metal sludge, comprising the steps of:
1) Collecting heavy metal sludge through a sludge collecting tank;
2) Conveying heavy metal sludge and a purifying agent into a stirring mixer through a first slurry pump, and stirring and uniformly mixing for 5-24 hours, wherein the stirring mixer adopts a positive rotation and reverse rotation alternating mode for stirring;
3) Conveying the heavy metal sludge after being stirred and mixed uniformly into a passivation pool, maintaining the temperature at 35-60 ℃ and the water content at 30-60%, and carrying out passivation treatment for 120-200 hours;
Wherein the purifying agent comprises quicklime and modified zeolite, and quicklime: the mass ratio of the modified zeolite is 1:1.5-5; the purification medicament is added to the input end of the first slurry pump through a first medicament adding device, and the purification medicament added through the first medicament adding device: the mass ratio of the heavy metal sludge is 1:6-15.
Preferably, the stirring mixer comprises a bracket, a stirring barrel and a first stirrer, wherein the stirring barrel is arranged on the bracket, and the first stirrer comprises a rotating shaft extending into the stirring barrel, a stirring paddle connected to the rotating shaft and positioned at the lower part in the stirring barrel, and a motor for driving the rotating shaft to rotate;
the stirring paddle is of a central symmetry structure and comprises a shaft sleeve and two crescent blades, wherein the shaft sleeve is used for being in driving connection with the rotating shaft, and the two crescent blades are connected to the shaft sleeve.
Preferably, the inner end of the blade is connected with the shaft sleeve, and the width and the height of the blade are gradually reduced from the inner end of the blade to the outer end direction of the blade;
The outer side surface and the inner side surface of the blade are respectively provided with a smooth curved surface, and the height of the upper surface of the blade is gradually reduced from the outer side surface of the blade to the inner side surface direction of the blade.
Preferably, the stirring mixer is further provided with a distributor, and the distributor comprises a feeding main pipe, a first feeding branch pipe and a second feeding branch pipe which are communicated with the feeding main pipe, a first electromagnetic valve arranged on the first feeding branch pipe and a second electromagnetic valve arranged on the second feeding branch pipe;
The first feeding branch pipe and the second feeding branch pipe are symmetrically arranged, and the tail ends of the first feeding branch pipe and the second feeding branch pipe are tangentially communicated with the barrel wall of the stirring barrel;
When the stirring mixer adopts a forward rotation mode to stir, the first electromagnetic valve is closed, the second electromagnetic valve is opened and closed, all heavy metal sludge enters the stirring barrel in a tangential direction through the second feeding branch pipe, and at the moment, the rotational flow direction formed by the heavy metal sludge entering in the tangential direction is the same as the forward rotation direction of the stirring mixer;
When the stirring mixer adopts a reversing mode to stir, the second electromagnetic valve is closed, the first electromagnetic valve is opened and closed, all heavy metal sludge enters the stirring barrel along the tangential direction through the first feeding branch pipe, and at the moment, the rotational flow direction formed by the heavy metal sludge entering the stirring mixer along the tangential direction is the same as the reversing direction of the stirring mixer.
Preferably, the stirring mixer is further provided with a second dosing device for supplementing the purifying agent, and the purifying agent added by the second dosing device is supplemented: the mass ratio of the heavy metal sludge is 1:12-30.
Preferably, the heavy metal sludge uniformly mixed by the stirring mixer is conveyed into the passivation pool through a second slurry pump.
Preferably, the preparation method of the modified zeolite comprises the following steps:
1) Adding natural zeolite into a mixture of inorganic acid and inorganic salt for soaking;
2) Filtering, discarding the filtrate, and cleaning the obtained soaked natural zeolite with deionized water;
3) Soaking the natural zeolite treated in the step 2) in cerium chloride solution at 50-80 ℃, filtering, discarding filtrate, and drying to obtain a modified zeolite precursor;
4) Drying the modified zeolite precursor at 100-200 ℃;
5) Adding the dried modified zeolite precursor and trimethylchlorosilane into a reaction vessel, stirring at room temperature for reaction for 2-5 hours, cleaning and drying to obtain the modified zeolite.
Preferably, the step 1) specifically includes: adding natural zeolite into mixed solution of hydrochloric acid, calcium chloride and ferric chloride, and soaking for 4-8 hr;
Wherein the natural zeolite is mordenite; in the mixed solution, the concentration of hydrochloric acid is 1-3mol/L, the concentration of calcium chloride is 0.2-0.8mol/L, and the concentration of ferric chloride is 0.4-1.6mol/L;
the concentration of the cerium chloride solution in the step 3) is 0.01-0.2mol/L.
Preferably, the step 5) specifically includes: adding the dried modified zeolite precursor and diethyl ether containing trimethylchlorosilane with the concentration of 10-50g/L into a reaction vessel, stirring at room temperature for reaction for 3 hours, transferring the reaction product to a sand core funnel, filtering, washing with acetone, and drying at 100-120 ℃ to obtain the modified zeolite.
Preferably, the method for purifying heavy metal sludge comprises the following steps:
1) Collecting heavy metal sludge through a sludge collecting tank;
2) The heavy metal sludge and the purifying agent added by the first dosing device are conveyed to a stirring mixer together through a first slurry pump, the purifying agent is added in a supplementary mode through a second dosing device, the heavy metal sludge and the purifying agent are stirred and mixed uniformly for 6 hours, and the stirring mixer is stirred in a circulating alternating mode of rotating forwards for 1 hour and rotating reversely for 0.5 hour;
Wherein, the quicklime in the purifying agent: the mass ratio of the modified zeolite is 1:3; purifying agent added by the first dosing device: the mass ratio of the heavy metal sludge is 1:8, and the added purifying agent is supplemented by the second dosing device: the mass ratio of the heavy metal sludge is 1:16;
3) And (3) conveying the heavy metal sludge after uniform stirring and mixing into a passivation pool, maintaining the temperature at 40 ℃ and the water content at 40%, and carrying out passivation treatment for 144 hours.
The beneficial effects of the invention are as follows:
The method for purifying the heavy metal sludge is simple to operate and low in cost, can efficiently purify heavy metal pollutants and organic pollutants in the sludge, can realize recycling of the sludge, and utilizes environmental protection;
According to the invention, through the cooperation of the stirring mixer, the distributor, the first slurry pump and the second slurry pump, the multiple stirring and mixing of the purifying agent and the sludge can be realized, so that the mixing effect of the agent and the sludge can be improved, and the purifying effect of the sludge is finally improved;
According to the invention, the modified zeolite and the quicklime are used together, so that the purification effect of heavy metals and organic pollutants in the sludge can be greatly improved.
Drawings
FIG. 1 is a schematic flow chart of the method for purifying heavy metal sludge of the present invention;
FIG. 2 is a schematic diagram of the structure of a stirring mixer employed in the method of the present invention;
FIG. 3 is a schematic top view of a first mixer used in the method of the present invention;
FIG. 4 is a schematic view of the structure of a stirring paddle used in the method of the present invention;
fig. 5 is a schematic view of another view of a stirring paddle used in the method of the present invention.
Reference numerals illustrate:
1-a sludge collection tank; 2-a first slurry pump; 3-a first dosing device; 4-stirring mixer; 5-a second dosing device; 6-a second slurry pump; 7, a passivation pool; 10-a second stirrer; 40-a bracket; 41-a stirring barrel; 42-a first stirrer; 43-a rotating shaft; 44-stirring paddles; 45-motor; 46-shaft sleeve; 47-blades; 410-a discharge gate; 470-inner end; 471-outer end; 472-outer side; 473-an inner side; 474-upper surface; 48-distributing device; 480-a main feeding pipe; 481-a first feed leg; 482-a second feed leg; 483—a first solenoid valve; 484-second solenoid valve.
Detailed Description
The present invention is described in further detail below with reference to examples to enable those skilled in the art to practice the same by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
Referring to fig. 1, the present embodiment provides a method for purifying heavy metal sludge, comprising the steps of:
1) Collecting heavy metal sludge through a sludge collecting tank 1;
2) The heavy metal sludge and the purifying agent are conveyed to a stirring mixer 4 through a first slurry pump 2 to be stirred and mixed uniformly for 5-24 hours, and the stirring mixer 4 adopts a positive rotation and reverse rotation alternating mode to stir;
3) Conveying the heavy metal sludge after being stirred and mixed evenly into a passivation pool 7, and carrying out passivation treatment for 120-200 hours under the conditions that the temperature is 35-60 ℃ and the water content is 30-60% (the mass of water accounts for the mass of the total sludge);
Wherein the purifying agent comprises quicklime and modified zeolite, and the quicklime: the mass ratio of the modified zeolite is 1:1.5-5; the purification agent is added to the input end of the first slurry pump 2 through the first dosing device 3, and the purification agent added through the first dosing device 3: the mass ratio of the heavy metal sludge is 1:6-15.
Heavy metals in the passivated sludge can generate stable metal compounds which cannot be leached out under the conventional environment, and the purified sludge can be recycled as soil restoration filler.
Referring to fig. 2 to 5, the stirrer-mixer 4 employed in the present embodiment comprises a bracket 40, a stirring vessel 41 and a first stirrer 42, the stirring vessel 41 being provided on the bracket 40, the first stirrer 42 comprising a rotary shaft 43 extending into the stirring vessel 41, a stirring paddle 44 connected to the rotary shaft 43 and located at a lower portion within the stirring vessel 41, and a motor 45 for driving the rotary shaft 43 to rotate;
the stirring paddle 44 has a central symmetrical structure, and comprises a shaft sleeve 46 for driving connection with the rotating shaft 43 and two crescent-shaped blades 47 connected to the shaft sleeve 46 (the shaft sleeve 46 is taken as the center, and the stirring paddle 44 can be overlapped with the original pattern after rotating 180 degrees). Further, the inner end 470 of the blade 47 is connected to the sleeve 46, and the width and height of the blade 47 gradually decrease from the inner end 470 of the blade 47 toward the outer end 471 of the blade 47; the outer side 472 and the inner side 473 of the blade 47 each have a smooth curved surface, and the height of the upper surface 474 of the blade 47 gradually decreases from the outer side 472 of the blade 47 toward the inner side 473 of the blade 47. Referring to the figures, the height of the blades 47 decreases gradually from the inner end 470 toward the outer end 471, the blades 47 being tapered; and from the outside to the inside, the upper surface 474 of the vane 47 is inclined downwardly. Through above-mentioned structural design, cooperation pivot 43 just reverses, can greatly improve stirring mixing effect, and the concrete principle is:
Referring to fig. 3, 4 and 5, when the stirring paddle 44 rotates forward (rotates clockwise), the force receiving surface of the blade 47 is mainly the outer side surface 472 of the blade 47, and the blade 47 contacts the sludge through the smooth arc-shaped outer side surface 472 to push the whole sludge to flow in the clockwise direction. Since the sludge can slide along the outer side 472 of the blade 47 toward the end of the blade 47, the resistance of the blade 47 can be reduced to a certain extent, and the blade 47 is prevented from being stuck, so that the sludge is preferably stirred by forward rotation when the overall resistance of the sludge is high at the beginning. The forward rotation process mainly realizes the integral stirring of the sludge, and the horizontal direction is obviously stronger than the vertical direction;
When the stirring paddle 44 rotates reversely (rotates clockwise), the stress surface of the blade 47 is mainly the inner side 473 of the blade 47, and when the blade 47 rotates, on one hand, the sludge between the inner side 473 of the blade 47 and the shaft sleeve 46 is pushed to rotate anticlockwise, and part of the sludge can flow in the vertical direction due to the extrusion action; on the other hand, since the outer ends 471 of the blades 47 are gradually widened and raised toward the inner ends 470, the blades 47 exert shearing and squeezing effects on the sludge, so that the sludge is gradually raised and moved upward along the upper surfaces 474 of the blades 47, thereby improving the stirring and mixing effect in the vertical direction. The forward rotation process can simultaneously realize the stirring of the whole sludge and the local horizontal and vertical directions, and can greatly improve the stirring effect, but the resistance of the blades 47 is large, so that the reverse rotation is suitable after the forward rotation is performed to loosen the sludge.
In this embodiment, the stirring mixer 4 is further provided with a distributor 48, and the distributor 48 includes a main feeding pipe 480, a first feeding branch pipe 481 and a second feeding branch pipe 482 which are communicated with the main feeding pipe 480, a first electromagnetic valve 483 provided on the first feeding branch pipe 481, and a second electromagnetic valve 484 provided on the second feeding branch pipe 482;
the first and second feeding branch pipes 481 and 482 are symmetrically disposed, and the ends of the first and second feeding branch pipes 481 and 482 are each in tangential communication with the tub wall of the stirring tub 41;
When the stirring mixer 4 adopts a forward rotation mode to stir, the first electromagnetic valve 483 is closed, the second electromagnetic valve 484 is opened and closed, all heavy metal sludge enters the stirring barrel 41 in the tangential direction through the second feeding branch pipe 482, and at the moment, the rotational flow direction formed by the heavy metal sludge entering in the tangential direction is the same as the forward rotation direction of the stirring mixer 4;
When the stirring mixer 4 is stirring in the reverse rotation mode, the second electromagnetic valve 484 is closed, the first electromagnetic valve 483 is opened and closed, all heavy metal sludge enters the stirring barrel 41 in the tangential direction through the first feeding branch pipe 481, and at this time, the rotational flow direction formed by the heavy metal sludge entering in the tangential direction is the same as the reverse rotation direction of the stirring mixer 4.
In this embodiment, heavy metal sludge is guided to enter the stirring barrel 41 along the tangential direction, and rotational flow is formed by utilizing the speed carried by the sludge, so that auxiliary rotational force can be provided for the stirring paddle 44, and forward stirring and reverse stirring of the stirring paddle 44 can be matched through two branch pipes and two matched electromagnetic valves. For example, when the mixer 4 is rotated forward (clockwise), the rotational flow discharged from the second feed pipe 482 is clockwise, thereby providing auxiliary power for mixing, improving the mixing effect and reducing the energy consumption. The lower part of the stirring tank 41 is also provided with a discharge gate 410, and the uniformly mixed sludge is discharged after the discharge gate 410 is opened.
In a preferred embodiment, the stirring mixer 4 is further provided with a second dosing device 5 for adding a purification agent, the added purification agent being added by the second dosing device 5: the mass ratio of the heavy metal sludge is 1:12-30. The treatment effect of the medicament can be improved by sectional dosing.
In a preferred embodiment, the heavy metal sludge after being mixed by the stirring mixer 4 is conveyed to the passivation tank 7 by the second slurry pump 6.
In a preferred embodiment, a second stirrer 10 is also provided in the sludge collection basin 1.
The mixing degree of the purifying agent and the heavy metal sludge has an important influence on the purifying effect, and the more the mixing is, the lower the utilization efficiency of the purifying agent is, and the more heavy metal substances in the sludge can be effectively purified. In the preferred embodiment, the purification medicament added by the first medicament adding device 3 and the heavy metal sludge can be uniformly mixed for the first time through the first slurry pump 2, the purification medicament added by the first medicament adding device 3 and the second medicament adding device 5 and the heavy metal sludge are uniformly mixed again in the stirring mixer 4, and then all the purification medicaments and the heavy metal sludge are uniformly mixed again through the second slurry pump 6, so that the mixing effect of the purification medicaments and the heavy metal sludge can be greatly improved through three times of mixing, and the treatment effect of the sludge can be improved.
The quicklime is used as a passivating agent to reduce the heavy metal content in the sludge and reduce the water content of the sludge, and the heat generated by the reaction of the quicklime and the water in the sludge can help to maintain the temperature requirement for passivation. However, the effect of purifying the sludge by using the quicklime alone is limited, so that the purification effect of heavy metals and some organic pollutants in the sludge can be greatly improved by adopting the modified zeolite and the quicklime to be matched.
In this example, the preparation method of the modified zeolite comprises the following steps:
1) Adding natural zeolite into a mixture of inorganic acid and inorganic salt for soaking;
2) Filtering, discarding the filtrate, and cleaning the obtained soaked natural zeolite with deionized water;
3) Soaking the natural zeolite treated in the step 2) in cerium chloride solution at 50-80 ℃, filtering, discarding filtrate, and drying to obtain a modified zeolite precursor;
4) Drying the modified zeolite precursor at 100-200 ℃;
5) Adding the dried modified zeolite precursor and trimethylchlorosilane into a reaction vessel, stirring at room temperature for reaction for 2-5 hours, cleaning and drying to obtain the modified zeolite.
Wherein, step 1) specifically includes: adding natural zeolite into mixed solution of hydrochloric acid, calcium chloride and ferric chloride, and soaking for 4-8 hr;
Wherein the natural zeolite is mordenite; in the mixed solution, the concentration of hydrochloric acid is 1-3mol/L, the concentration of calcium chloride is 0.2-0.8mol/L, and the concentration of ferric chloride is 0.4-1.6mol/L;
The concentration of the cerium chloride solution in the step 3) is 0.01-0.2mol/L.
Wherein, step 5) specifically includes: adding the dried modified zeolite precursor and diethyl ether containing trimethylchlorosilane with the concentration of 10-50g/L into a reaction vessel, stirring at room temperature for reaction for 3 hours, transferring the reaction product to a sand core funnel, filtering, washing with acetone, and drying at 100-120 ℃ to obtain the modified zeolite. The modified zeolite is crushed to the required size and shape when in use.
The natural zeolite is an aluminosilicate mineral with a porous structure, has stable property, large specific surface area and good adsorption performance, but the natural zeolite has limited adsorption capacity and poor adsorption effect on a plurality of organic matters and heavy metals. According to the invention, the natural zeolite is modified, so that the adsorption effect of the natural zeolite on organic matters and heavy metal ions can be greatly improved, the natural zeolite can be used for purifying sludge, and the content of the heavy metals and the organic matters in the treated sludge can be greatly reduced.
The natural zeolite is subjected to acid leaching treatment by hydrochloric acid, so that amorphous substances in zeolite pore canals can be dissolved, the pore canal resistance is reduced, the effective space of the pore canal is widened by replacing cations with large radius in the zeolite pore canals, and the adsorption capacity of the zeolite is increased; on the other hand, the zeolite framework can be dealuminated, and the stability and adsorption capacity of the zeolite can be improved. Meanwhile, calcium chloride and ferric chloride are mixed in the hydrochloric acid, and the ion exchange capacity of zeolite can be increased by soaking inorganic salt, so that the adsorption performance and cation exchange performance of natural zeolite are improved, the ferric chloride can promote ion exchange, and the speed of ion exchange reaching a dynamic balance state is accelerated. The adsorption performance and stability of the zeolite can be comprehensively improved by soaking the natural zeolite by the mixed solution of hydrochloric acid, calcium chloride and ferric chloride.
The natural zeolite is soaked in cerium chloride solution, rare earth cerium is utilized to further modify the natural zeolite, and the surface of the modified zeolite is covered with hydroxyl groups, so that heavy metal cations and anions are easy to generate surface coordination complexes, and the adsorption performance of the zeolite on the heavy metal cations and anions can be improved.
Finally, the surface of the zeolite is modified by adopting trimethylchlorosilane, and the trimethylchlorosilane reacts with terminal silicon hydroxyl groups on the surface of the zeolite to ensure that the zeolite has a good hydrophobic surface, so that organic matters can be adsorbed well; and because the trimethylchlorosilane molecules are larger than the pore diameters of the zeolite, the trimethylchlorosilane is modified on the outer surface of the zeolite, and the hydrophilic surface in the pore canal of the zeolite is not influenced, so that the modified zeolite shows bipolar properties, organic matters can be adsorbed on the hydrophobic surface, metal ions can be adsorbed on the hydrophilic pore canal, various pollutants in the sludge can be purified, and finally the adsorption performance of the zeolite can be greatly improved. And the modified zeolite can form stable compounds after adsorbing metal ions and organic matters, and can not be leached in a conventional environment.
Example 2
This example was further modified based on example 1, and the same as example 1 was mostly given, and only different parts are listed below.
The embodiment provides a method for purifying heavy metal sludge, which comprises the following steps:
1) Collecting heavy metal sludge through a sludge collecting tank 1;
2) The heavy metal sludge and the purifying agent added by the first dosing device 3 are conveyed to the stirring mixer 4 together through the first slurry pump 2, the purifying agent is added by the second dosing device 5, the mixture is stirred and mixed for 6 hours, and the stirring mixer 4 adopts a circulation alternating mode of rotating for 1 hour in the forward direction and rotating for 0.5 hour in the reverse direction;
wherein, the quicklime in the purifying agent: the mass ratio of the modified zeolite is 1:3; purifying agent added by the first dosing device 3: the mass ratio of the heavy metal sludge is 1:8, and the added purifying agent is supplemented by the second dosing device 5: the mass ratio of the heavy metal sludge is 1:16;
3) And (3) conveying the heavy metal sludge after uniform stirring and mixing into a passivation tank 7, maintaining the temperature at 40 ℃ and the water content at 40%, and carrying out passivation treatment for 144 hours.
Wherein the preparation method of the modified zeolite comprises the following steps:
1) Adding natural zeolite into mixed solution of hydrochloric acid, calcium chloride and ferric chloride, and soaking for 6 hours;
Wherein the natural zeolite is mordenite; in the mixed solution, the concentration of hydrochloric acid is 1.5mol/L, the concentration of calcium chloride is 0.4mol/L, and the concentration of ferric chloride is 0.6mol/L;
2) Filtering, discarding the filtrate, and cleaning the obtained soaked natural zeolite with deionized water;
3) Soaking the natural zeolite treated in the step 2) in cerium chloride solution at 60 ℃, filtering, discarding the filtrate, and drying to obtain a modified zeolite precursor; wherein the concentration of the cerium chloride solution is 0.01mol/L.
4) Drying the modified zeolite precursor at 150 ℃;
5) Adding the dried modified zeolite precursor and diethyl ether containing trimethylchlorosilane with the concentration of 25g/L into a reaction vessel, stirring at room temperature for reaction for 3 hours, transferring the reaction product to a sand core funnel, carrying out suction filtration, washing with acetone, and drying at 110 ℃ to obtain the modified zeolite. The modified zeolite is crushed to a diameter of 1mm or less.
Example 3
This example was further modified based on example 1, and the same as example 1 was mostly given, and only different parts are listed below.
The embodiment provides a method for purifying heavy metal sludge, which comprises the following steps:
1) Collecting heavy metal sludge through a sludge collecting tank 1;
2) The heavy metal sludge and the purifying agent added by the first dosing device 3 are conveyed to the stirring mixer 4 together through the first slurry pump 2, the purifying agent is added by the second dosing device 5, the mixture is stirred and mixed for 6 hours, and the stirring mixer 4 adopts a circulation alternating mode of rotating for 1 hour in the forward direction and rotating for 0.5 hour in the reverse direction;
Wherein, the quicklime in the purifying agent: the mass ratio of the modified zeolite is 1:3.5; purifying agent added by the first dosing device 3: the mass ratio of the heavy metal sludge is 1:7, and the added purifying agent is supplemented by the second dosing device 5: the mass ratio of the heavy metal sludge is 1:20;
3) And (3) conveying the heavy metal sludge after uniform stirring and mixing into a passivation tank 7, maintaining the temperature at 40 ℃ and the water content at 40%, and carrying out passivation treatment for 168 hours.
Example 4
The preparation method of the modified zeolite comprises the following steps:
1) Adding natural zeolite into mixed solution of hydrochloric acid, calcium chloride and ferric chloride, and soaking for 6 hours;
wherein the natural zeolite is mordenite; in the mixed solution, the concentration of hydrochloric acid is 2.5mol/L, the concentration of calcium chloride is 0.7mol/L, and the concentration of ferric chloride is 1.2mol/L;
2) Filtering, discarding the filtrate, and cleaning the obtained soaked natural zeolite with deionized water;
3) Soaking the natural zeolite treated in the step 2) in cerium chloride solution at 60 ℃, filtering, discarding the filtrate, and drying to obtain a modified zeolite precursor; wherein the concentration of the cerium chloride solution is 0.03mol/L.
4) Drying the modified zeolite precursor at 150 ℃;
5) Adding the dried modified zeolite precursor and diethyl ether containing trimethylchlorosilane with the concentration of 35g/L into a reaction vessel, stirring at room temperature for reaction for 3 hours, transferring the reaction product to a sand core funnel, carrying out suction filtration, washing with acetone, and drying at 110 ℃ to obtain the modified zeolite. The modified zeolite is crushed to a diameter of 1mm or less.
Example 5
The dewatered sludge from a sewage treatment plant in su zhou was purified by the method of example 2. The basic properties of the dewatered sludge are shown in table 1 below:
TABLE 1
| Moisture content/% | Cu/mg·kg-1 | Zn/mg·kg-1 | Pb/mg·kg-1 | Cd/mg·kg-1 | COD/mg·kg-1 |
| 68 | 73 | 105 | 54 | 41 | 1420 |
The sludge (water content is 56%) treated by the method of example 2 is laid on a non-woven fabric with a thickness of 4-7cm, watered on a sludge layer, and the percolated water below the sludge layer is collected, and the quality of the percolated water is analyzed, and the analysis results are shown in the following table 2:
TABLE 2
| Cu/mg·L-1 | Zn/mg·L-1 | Pb/mg·L-1 | Cd/mg·L-1 | COD/mg·L-1 |
| 5 | 8 | 2.2 | 1.3 | 27 |
As can be seen from the comparison of the results in Table 2 and Table 1, the treatment of the method in example 2 can realize the effective fixation of heavy metals and organic pollutants, and the contents of the heavy metals and the organic pollutants in the water seepage are very low, which indicates that the method can realize the efficient purification of heavy metal sludge.
Comparative example 1
The treatment method was substantially the same as in example 2, except that: without stirring by the stirring mixer 4, all the purifying agent is added into the sludge collecting tank 1, and then the sludge is directly conveyed to the passivation tank 7 by the first slurry pump 2 for treatment (excluding the second slurry pump 6).
Comparative example 2
The treatment method was substantially the same as in example 2, except that: modified zeolite is not included in the purification agent.
Comparative example 3
The treatment method was substantially the same as in example 2, except that: the purifying agent comprises quicklime and natural mordenite.
The same method as in comparative examples 1 to 3 was used to treat sludge of the same origin as in example 5, and the treated sludge was subjected to a water seepage test in the same manner as in example 5, and the quality of the percolated water was analyzed, and the analysis results are shown in Table 3 below:
TABLE 3 Table 3
| Cu/mg·L-1 | Zn/mg·L-1 | Pb/mg·L-1 | Cd/mg·L-1 | COD/mg·L-1 | |
| Comparative example 1 | 32 | 44 | 26 | 19.4 | 463 |
| Comparative example 2 | 37 | 49 | 33.6 | 22.5 | 987 |
| Comparative example 3 | 21 | 27 | 15.2 | 12.6 | 233 |
As can be seen from the comparison of the results in table 3 and table 2, the present invention can significantly improve the purification effect of the sludge by using the stirring mixer4 to sufficiently stir the purifying agent and the sludge; by adopting the modified zeolite, the fixing effect of heavy metals and organic pollutants in the sludge can be greatly improved, and the purification of the sludge is realized.
Although embodiments of the present invention have been disclosed above, it is not limited to the use of the description and embodiments, it is well suited to various fields of use for the invention, and further modifications may be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the particular details without departing from the general concepts defined in the claims and the equivalents thereof.
Claims (8)
1. A method for purifying heavy metal sludge, comprising the steps of:
1) Collecting heavy metal sludge through a sludge collecting tank;
2) The heavy metal sludge and the purifying agent are conveyed to a stirring mixer together through a first slurry pump to be stirred and mixed uniformly for 5-24 hours, and the stirring mixer adopts a positive rotation and reverse rotation alternating mode to stir;
3) Conveying the heavy metal sludge after being stirred and mixed uniformly into a passivation pool, maintaining the temperature at 35-60 ℃ and the water content at 30-60%, and carrying out passivation treatment for 120-200 hours;
Wherein the purifying agent comprises quicklime and modified zeolite, and quicklime: the mass ratio of the modified zeolite is 1:1.5-5; the purification medicament is added to the input end of the first slurry pump through a first medicament adding device, and the purification medicament added through the first medicament adding device: the mass ratio of the heavy metal sludge is 1:6-15;
The stirring mixer comprises a bracket, a stirring barrel and a first stirrer, wherein the stirring barrel is arranged on the bracket, and the first stirrer comprises a rotating shaft extending into the stirring barrel, a stirring paddle connected to the rotating shaft and positioned at the lower part in the stirring barrel, and a motor for driving the rotating shaft to rotate;
the stirring paddle is of a central symmetrical structure and comprises a shaft sleeve and two crescent-shaped blades, wherein the shaft sleeve is used for being in driving connection with the rotating shaft, and the two crescent-shaped blades are connected to the shaft sleeve;
the inner ends of the blades are connected with the shaft sleeve, and the width and the height of the blades are gradually reduced from the inner ends of the blades to the outer ends of the blades;
The outer side surface and the inner side surface of the blade are respectively provided with a smooth curved surface, and the height of the upper surface of the blade is gradually reduced from the outer side surface of the blade to the inner side surface direction of the blade.
2. The method for purifying heavy metal sludge according to claim 1, wherein a distributor is further provided on the stirring mixer, the distributor including a main feeding pipe, a first feeding branch pipe and a second feeding branch pipe communicating with the main feeding pipe, a first electromagnetic valve provided on the first feeding branch pipe, and a second electromagnetic valve provided on the second feeding branch pipe;
The first feeding branch pipe and the second feeding branch pipe are symmetrically arranged, and the tail ends of the first feeding branch pipe and the second feeding branch pipe are tangentially communicated with the barrel wall of the stirring barrel;
When the stirring mixer adopts a forward rotation mode to stir, the first electromagnetic valve is closed, the second electromagnetic valve is opened and closed, all heavy metal sludge enters the stirring barrel in a tangential direction through the second feeding branch pipe, and at the moment, the rotational flow direction formed by the heavy metal sludge entering in the tangential direction is the same as the forward rotation direction of the stirring mixer;
When the stirring mixer adopts a reversing mode to stir, the second electromagnetic valve is closed, the first electromagnetic valve is opened and closed, all heavy metal sludge enters the stirring barrel along the tangential direction through the first feeding branch pipe, and at the moment, the rotational flow direction formed by the heavy metal sludge entering the stirring mixer along the tangential direction is the same as the reversing direction of the stirring mixer.
3. The method of purifying heavy metal sludge according to claim 2, wherein the stirring mixer is further provided with a second dosing device for supplementing the purifying agent, and the purifying agent added is supplemented by the second dosing device: the mass ratio of the heavy metal sludge is 1:12-30.
4. A method for purifying heavy metal sludge according to claim 3, wherein the heavy metal sludge homogenized by the stirring mixer is transported to the passivation tank by a second slurry pump.
5. A method for purifying heavy metal sludge according to claim 3, wherein the preparation method of the modified zeolite comprises the steps of:
1) Adding natural zeolite into a mixture of inorganic acid and inorganic salt for soaking;
2) Filtering, discarding the filtrate, and cleaning the obtained soaked natural zeolite with deionized water;
3) Soaking the natural zeolite treated in the step 2) in cerium chloride solution at 50-80 ℃, filtering, discarding filtrate, and drying to obtain a modified zeolite precursor;
4) Drying the modified zeolite precursor at 100-200 ℃;
5) Adding the dried modified zeolite precursor and trimethylchlorosilane into a reaction vessel, stirring at room temperature for reaction for 2-5 hours, cleaning and drying to obtain the modified zeolite.
6. The method for purifying heavy metal sludge according to claim 5, wherein the step 1) specifically comprises: adding natural zeolite into the mixed solution of hydrochloric acid, calcium chloride and ferric chloride, and soaking for 4-8 hours;
Wherein the natural zeolite is mordenite; in the mixed solution, the concentration of hydrochloric acid is 1-3mol/L, the concentration of calcium chloride is 0.2-0.8mol/L, and the concentration of ferric chloride is 0.4-1.6mol/L;
the concentration of the cerium chloride solution in the step 3) is 0.01-0.2mol/L.
7. The method for purifying heavy metal sludge according to claim 5, wherein the step 5) specifically comprises: adding the dried modified zeolite precursor and diethyl ether containing trimethylchlorosilane with the concentration of 10-50 g/L into a reaction vessel, stirring at room temperature for reaction for 3 hours, transferring the reaction product to a sand core funnel, filtering, washing with acetone, and drying at 100-120 ℃ to obtain the modified zeolite.
8. The method for purifying heavy metal sludge according to any one of claims 3 to 7, comprising the steps of:
1) Collecting heavy metal sludge through a sludge collecting tank;
2) The heavy metal sludge and the purifying agent added by the first dosing device are conveyed to a stirring mixer together through a first slurry pump, the purifying agent is added in a supplementary mode through a second dosing device, the heavy metal sludge and the purifying agent are stirred and mixed uniformly for 6 hours, and the stirring mixer is stirred in a circulating alternating mode of rotating forwards for 1 hour and rotating reversely for 0.5 hour;
Wherein, the quicklime in the purifying agent: the mass ratio of the modified zeolite is 1:3; purifying agent added by the first dosing device: the mass ratio of the heavy metal sludge is 1:8, and the added purifying agent is supplemented by the second dosing device: the mass ratio of the heavy metal sludge is 1:16;
3) And (3) conveying the heavy metal sludge after uniform stirring and mixing into a passivation pool, maintaining the temperature at 40 ℃ and the water content at 40%, and carrying out passivation treatment for 144 hours.
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