CN111807596B - Process method for treating precipitated white carbon black wastewater - Google Patents
Process method for treating precipitated white carbon black wastewater Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 239000002351 wastewater Substances 0.000 title claims abstract description 119
- 239000006229 carbon black Substances 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 75
- 230000008569 process Effects 0.000 title claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 103
- 239000012528 membrane Substances 0.000 claims abstract description 64
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 61
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 56
- 239000010703 silicon Substances 0.000 claims abstract description 56
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 44
- 238000001704 evaporation Methods 0.000 claims abstract description 38
- 230000008020 evaporation Effects 0.000 claims abstract description 38
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 50
- 239000000377 silicon dioxide Substances 0.000 claims description 31
- 238000004519 manufacturing process Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 15
- 239000010802 sludge Substances 0.000 claims description 13
- 239000000701 coagulant Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000002455 scale inhibitor Substances 0.000 claims description 12
- 239000003638 chemical reducing agent Substances 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000004062 sedimentation Methods 0.000 claims description 6
- AOSFMYBATFLTAQ-UHFFFAOYSA-N 1-amino-3-(benzimidazol-1-yl)propan-2-ol Chemical group C1=CC=C2N(CC(O)CN)C=NC2=C1 AOSFMYBATFLTAQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 238000004069 wastewater sedimentation Methods 0.000 claims description 3
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 claims 1
- 230000000903 blocking effect Effects 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 description 28
- 238000005189 flocculation Methods 0.000 description 22
- 230000016615 flocculation Effects 0.000 description 17
- 238000001556 precipitation Methods 0.000 description 17
- 238000000926 separation method Methods 0.000 description 14
- 230000000694 effects Effects 0.000 description 11
- 238000004065 wastewater treatment Methods 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 239000013043 chemical agent Substances 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 229910000000 metal hydroxide Inorganic materials 0.000 description 6
- 238000005868 electrolysis reaction Methods 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000008119 colloidal silica Substances 0.000 description 4
- 239000012452 mother liquor Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 229920002401 polyacrylamide Polymers 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 150000004692 metal hydroxides Chemical class 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 3
- 229960001866 silicon dioxide Drugs 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000012744 reinforcing agent Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229960004029 silicic acid Drugs 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000001687 destabilization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 238000005188 flotation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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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
-
- 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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
- C02F11/125—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering using screw filters
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2001/007—Processes including a sedimentation step
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- C02F2101/101—Sulfur compounds
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- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
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Abstract
The invention discloses a process method for treating precipitated white carbon black wastewater, which comprises the following steps: carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater by using an electric desiliconization device; carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water; performing reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water; and sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate. Experiments prove that compared with the prior art, the process method disclosed by the invention can effectively remove soluble silicon in the precipitated white carbon black wastewater, well solves the problem of scaling and blocking of an ultrafiltration membrane and a reverse osmosis membrane, greatly prolongs the service time of the membrane, reduces the treatment cost and realizes zero discharge of the precipitated white carbon black wastewater.
Description
Technical Field
The application relates to the technical field of chemical wastewater treatment, and more particularly relates to a process method for treating precipitated white carbon black wastewater.
Background
White carbon black is the common name of synthetic hydrated silica powder, and the name of white carbon black is derived from the fact that white carbon black has the performance similar to that of carbon black for reinforcing rubber. Carbon black has a long history as a reinforcing agent for rubber, and since carbon black has been limited to some applications requiring color as a black reinforcing agent, studies have been made to replace carbon black with chemically synthesized active amorphous silica. Amorphous silica is another excellent reinforcing filler, following carbon black, and is customarily referred to as white carbon, because of its white color.
The white carbon black is mainly divided into precipitated white carbon black and gas-phase white carbon black according to the production method, wherein the precipitated white carbon black is commonly called white smoke, the chemical name of the precipitated white carbon black is precipitated hydrated silicon dioxide, and the molecular formula of the precipitated white carbon black is SiO2·nH2O, since n is indefinite, white carbon black also has no fixed molecular weight. The synthesis process of precipitated silica is essentially the process of converting dense crystalline silica (quartz sand) into loose amorphous hydrated silica, i.e. SiO2→SiO2·nH2And O. The specific process can be mainly divided into the traditional precipitation method and the gel method, wherein the traditional precipitation method is to obtain loose and finely dispersed SiO precipitated in a flocculent structure by acidifying the silicate2The method has the advantages of easily available raw materials, simple production flow, low energy consumption and low investment. The main raw materials for producing the white carbon black by the traditional precipitation method are liquid water glass and sulfuric acid, and the specific process route is as follows: after the liquid water glass is prepared into a certain concentration, the liquid water glass and sulfuric acid with a certain concentration are respectively sent to a high-level tank, added into a reaction kettle at a certain speed and reacted at a certain temperature. And (3) delivering the reaction finished solution to a curing tank for curing for a certain time, pressurizing by a feeding pump, delivering the solution to a plate-and-frame filter press for separation, cleaning the separated filter cake with clear water, pulping, and delivering the filter cake to a drying tower for drying to obtain the powdery white carbon black product.
In the traditional precipitation method white carbon black production process, two kinds of waste water can appear, the first kind is white carbon black mother liquor (waste water), the mother liquor amount is about 8m for carrying out the year/t white carbon black, wherein the content of sodium sulfate is about 5.79%; the second method is white carbon black washing water (wastewater), the washing water amount is about 17 m/t white carbon black, and the sodium sulfate content is about 0.656%. The total amount of wastewater obtained after mixing mother liquor and washing water is 25 m/t of white carbon black, and the average content of sodium sulfate is about 2.559%. Meanwhile, the white carbon black mother liquor and the washing wastewater also contain colloidal silica, soluble silicon and other element substances through detection, and the table 1 shows the detection content of part of the element substances in the precipitated white carbon black wastewater.
TABLE 1
The prior art mainly comprises two methods for treating the precipitated white carbon black wastewater. The first method employs direct evaporation, and has the disadvantages of large investment and high operation cost. No matter the production system of 30000 tons of precipitated white carbon black produced in one year adopts multi-effect direct evaporation or MVR direct evaporation, the one-time investment is more than 6000 ten thousand yuan, the cost of each ton of white carbon black is increased by more than 800 yuan, which accounts for about 30% of the production cost, and the production system is unacceptable for production enterprises. The second method adopts membrane separation concentration and evaporation, and because the precipitated white carbon black wastewater contains a certain amount of silicon dioxide, mainly colloidal silicon and soluble silicon, especially because of the existence of the soluble silicon, silica scale can be formed on the membrane after the membrane separation equipment operates for several hours, so that silicon blockage is caused. No matter the ultrafiltration membrane or the reverse osmosis membrane is used, once the silicon plug is formed, the prior art means cannot be cleaned, and only a new membrane can be discarded and replaced, so that a pure membrane separation and concentration mode is fundamentally infeasible. Even if the flocculation precipitation is carried out by adding the chemical silicon removal agent before the membrane separation, the soluble silicon in the wastewater cannot be fully removed, and in addition, the chemical silicon removal agent has high cost, and enterprises cannot bear high operating cost, so far, no production enterprise at home and abroad really realizes the zero discharge of the white carbon black wastewater treatment.
From the above, how to provide a low-cost method for treating precipitated silica wastewater to achieve zero discharge of precipitated silica wastewater treatment is a technical problem to be solved urgently at present.
Disclosure of Invention
Because current sediment white carbon black waste water treatment technique, there is the processing apparatus to require highly, the investment is big, the problem that treatment cost is expensive, can't satisfy manufacturing enterprise's demand to realize sediment white carbon black waste water treatment "zero" and discharge. Therefore, the invention provides a process method for treating precipitated silica wastewater, which comprises the following steps:
carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater by using an electric desiliconization device;
carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water;
carrying out reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water;
and sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate.
Preferably, the method further comprises:
adding a silicon removing agent, a coagulant aid and a reducing agent into the wastewater after electrolytic silicon removal before the ultrafiltration treatment.
Further, the silicon removing agent is FeCl3The dosage is 0.01-0.1kg/t water; the coagulant aid is PAM, and the dosage is 0.001-0.005kg/t water; the reducing agent is ammonium bisulfite, and the dosage is 0.001-0.005kg/t water.
Preferably, the method further comprises:
adding a high silica scale inhibitor to the ultrafiltration treatment water prior to the reverse osmosis treatment.
Further, the high-silicon scale inhibitor is organic phosphate, and the using amount of the high-silicon scale inhibitor is 0.001-0.003kg/t of water.
Preferably, the pretreatment specifically comprises:
cooling precipitated white carbon black wastewater from a workshop wastewater tank by a wastewater cooling tower;
sending the cooled wastewater to a wastewater sedimentation tank for natural sedimentation;
and adding a small amount of alkali into the naturally settled wastewater to neutralize the wastewater to be neutral.
Preferably, the method further comprises:
and (4) conveying flocculate obtained after the ultrafiltration treatment to a sludge tank, and separating dewatered sludge by using a screw stacking machine.
Preferably, the method further comprises:
and sending the evaporation condensed water of the evaporation system and the clean water to a clean water tank for a white carbon black production system to use.
The invention discloses a process method for treating precipitated white carbon black wastewater, which comprises the following steps: carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater by using an electric desiliconization device; carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water; performing reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water; and sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate. Experiments prove that compared with the prior art, the process method disclosed by the invention can effectively remove soluble silicon in the precipitated white carbon black wastewater, well solves the problem of scaling and blocking of an ultrafiltration membrane and a reverse osmosis membrane, greatly prolongs the service time of the membrane, reduces the treatment cost and realizes zero discharge of the precipitated white carbon black wastewater.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow chart illustrating a process for treating precipitated silica wastewater according to an embodiment of the present invention;
FIG. 2 is a schematic diagram illustrating a structure of an electrical desiliconization apparatus according to an embodiment of the present invention.
Reference numerals: 1. a water inlet; 2. a water outlet; 3. a sewage draining outlet; 4. an electrode plate anode interface; 5. and an electrode plate cathode interface.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In the prior art, pure chemical silicon removal modes such as aluminum salt (PAC flocculant + PAM coagulant aid) and the like are generally adopted for treating white carbon black wastewater, and although the pure chemical silicon removal modes have a certain removal effect on colloidal silicon, the removal efficiency on soluble silicon is extremely low, so that a large amount of soluble silicon enters a subsequent ultrafiltration membrane and a reverse osmosis membrane, and silica scale is formed on the surface of the membrane after hours to pollute the plugging membrane. In the current technology, the best method for cleaning silicon dioxide pollution is to clean with hydrofluoric acid, but the use of hydrofluoric acid cleaning can cause irreparable damage to the film, so once the film forms a silicon plug, the film cannot be cleaned at all in actual operation, only a new film can be replaced, and the cost is too high due to the use of a large amount of chemical silicon removal agents, and enterprises cannot bear high operating cost. Therefore, no matter which treatment method is adopted for precipitated white carbon black wastewater in the prior art, the high operation cost of wastewater treatment is difficult to avoid, so that production enterprises cannot really realize zero discharge of white carbon black wastewater treatment.
In order to solve the technical problem, as shown in fig. 1, the invention discloses a process method for treating precipitated silica wastewater, which specifically comprises the following steps:
carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater by using an electric desiliconization device;
carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water;
performing reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water;
and sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate.
Specifically, the invention utilizes the electrolytic chemical flocculation technology to remove colloidal silica and soluble silica (electrical desiliconization or electrolytic desiliconization for short) in the precipitated white carbon black wastewater. The electric desiliconization device (see figure 2) is desiliconization equipment which is designed according to the electrochemical electrolysis principle and mainly comprises an electrolytic container and a bracket, wherein the bracket is arranged below the electrolytic container and plays a role in supporting and fixing. Two sides in the electrolytic container are respectively provided with a metal electrode plate which is respectively used as a cathode and an anode, and the middle part of the electrolytic container is provided with an electrode plate anode interface and an electrode plate cathode interface which correspond to the metal electrode plates and are used for supplying power to the metal electrode plates. The middle part of the electrolytic container is provided with a wastewater inlet, the precipitated white carbon black wastewater enters the electric desiliconization equipment for electrolytic desiliconization, and the optimal position of the water inlet is in the same horizontal line or lower than the horizontal line with the lower end of the metal electrode plate, so that the wastewater can be fully subjected to electrolytic desiliconization. The top end of the electrolytic container is provided with a water outlet for discharging the waste water after electrolytic treatment so as to enter the next working procedure. The lower end of the electrolytic vessel is provided with a sewage outlet, and pollutants flocculated and precipitated after electrolysis are discharged to a sludge tank. The working principle of the electric desiliconization device is as follows: the metal is used as an electrode, the white carbon black wastewater is electrolyzed between the electrode plates, chemical substances generated by the metal electrode during electrolysis and colloidal silicon and soluble silicon in the white carbon black wastewater generate a series of complex electrochemical reactions, or are removed by oxidation, or are separated out by dissociation, or are taken out of a water body by secondary gas, or are subjected to reduction reaction and the like, and finally the removal of the colloidal silicon and the soluble silicon is realized.
In a specific implementation scenario, the specific flow of the electrolytic silicon removal treatment is briefly described as follows: under the condition of certain current and voltage, Fe dissolved out of the metal anode2+、Al3+(the preferred use of Fe dissolution in the present invention2+Electrochemical device) plasma is hydrolyzed in water to generate flocculation, and H is generated by the anode and the cathode2And O2The air bubbles in the air flow are equal to each other, so that good air floating effect is generated, and O is generated2The oxidation effect is also realized on colloidal silica, soluble silica and other pollutants to be removed in the white carbon black wastewater. Colloidal silica and soluble silica in the white carbon black wastewater treated by the electrolytic chemical flocculation equipment are changed into flocs such as metal oxides, hydroxides and the like, so that the flocs are removed by a precipitation mode.
In order to remove flocs such as metal oxides and hydroxides formed by electrolytic desiliconization more conveniently and effectively, in a preferred embodiment of the present invention, a desiliconization agent, a coagulant aid and a reducing agent are added to the wastewater after electrolytic desiliconization after the electrolytic desiliconization and before the ultrafiltration.
Specifically, flocs such as metal oxides and hydroxides formed by electrolytic desiliconization are matched with a small amount of desiliconization agent, coagulant aid and reducing agent (or other auxiliaries with the same action), so that the specific surface area of the particles of the flocs is increased, the activity is improved, the stability is good, and the precipitation effect is better. Preferably, the silicon removing agent is FeCl3The dosage is 0.01-0.1kg/t water; what is needed isThe coagulant aid is PAM (polyacrylamide), and the dosage is 0.001-0.005kg/t water; the reducing agent is ammonium bisulfite, and the dosage is 0.001-0.005kg/t water. The addition amounts of the silicon removing agent, the coagulant aid and the reducing agent are far lower than the addition amount of the traditional chemical agent for removing silicon, so that the cost is reduced, and the secondary pollution is avoided. It should be noted that the dosage units of the chemical agents of the present invention are calculated based on the amount of wastewater actually treated.
At present, in the white carbon black industry, pure chemical agents are adopted to remove silicon in the research process of white carbon black precipitation wastewater treatment, and the white carbon black precipitation wastewater treatment is realized by improving membrane separation equipment. The invention breaks the existing thinking of precipitated white carbon black wastewater treatment, utilizes an electric desiliconization mode or a method combining electric desiliconization and chemical agents, and not only greatly reduces the treatment cost but also realizes the initiation of zero discharge of the precipitated white carbon black wastewater treatment through the mutual synergistic effect of electric desiliconization, chemical desiliconization, membrane separation and evaporation.
In order to improve the effect of the electrolytic silicon removal treatment, in a preferred embodiment of the present invention, before the electrolytic silicon removal treatment, the precipitated silica wastewater needs to be pretreated, and the pretreatment specifically includes:
cooling precipitated white carbon black wastewater from a workshop wastewater tank by a wastewater cooling tower;
sending the cooled wastewater to a wastewater sedimentation tank for natural sedimentation;
and adding a small amount of alkali into the naturally settled wastewater to neutralize the wastewater to be neutral.
Specifically, white carbon black wastewater containing sodium sulfate produced in the white carbon black production process by a precipitation method enters a workshop wastewater tank, the temperature of the wastewater is usually about 70 ℃, the wastewater is sent to a wastewater cooling tower for cooling treatment by a hot water pump, the wastewater enters a precipitation wastewater tank for natural precipitation after the temperature of the wastewater is reduced to below 40 ℃, and the wastewater after the impurities and part of precipitates are removed by precipitation is sent to an electric desiliconization device by the wastewater pump. Because the pH value of the wastewater is about 4.5 and is not suitable for electrolysis, a small amount of alkali needs to be added to neutralize the wastewater to be neutral before the wastewater enters the electric desiliconization device, and the electrolyzed metal hydroxide makes the wastewater tend to be alkalescent in the flocculation process, which is more beneficial to flocculation and precipitation of the wastewater.
The invention utilizes the immersed ultrafiltration membrane component to separate flocculate from the saline water to obtain ultrafiltration treated water. After the white carbon black wastewater is subjected to electric desiliconization, flocculation and precipitation, the rest suspended matters containing silicide are remained, and then most of silicide in the water can be removed through a subsequent immersed ultrafiltration membrane component. The immersed ultrafiltration membrane component is membrane separation equipment adopting an immersed ultrafiltration membrane (preferably a patent product CN 206828149U), can be directly immersed in a water tank, and can be flushed by air disturbance, so that the ultrafiltration membrane can still stably run when the concentration of suspended matters in the white carbon black wastewater reaches 1-2%. Meanwhile, the immersed ultrafiltration component adopts a unique slotted design, so that the suspended matters containing silicide which are left after the electric desiliconization flocculation precipitation can be quickly separated from the membrane component and can not be accumulated in the ultrafiltration membrane, the influence of the adhesion on the surface of the membrane on the filtration effect is avoided, and the flux of the membrane is ensured. Therefore, the immersed ultrafiltration membrane component has stronger impact resistance to the water quality fluctuation of the white carbon black wastewater, can not be blocked after long-time operation, and also overcomes the problem of incomplete flocculation reaction of the traditional ultrafiltration membrane because the retention time of suspended matters in the membrane pool is prolonged. And the immersed ultrafiltration membrane component and the electric desiliconization device are cooperatively used and applied to the treatment of the precipitated white carbon black wastewater, so that the soluble silicon in the wastewater is greatly removed, and the subsequent treatment method of reverse osmosis and evaporation is ensured to be smoothly carried out.
In order to fully recover and treat the white carbon black wastewater, in a preferred embodiment of the invention, flocs obtained after the ultrafiltration treatment are sent to a sludge tank, and dewatered sludge is separated by a screw stacking machine. Specifically, after silicon in the wastewater passing through the electric desiliconization device is flocculated by adding agents such as a desiliconization agent, a coagulant aid and the like, the wastewater enters an immersed ultrafiltration membrane assembly to separate flocculate from saline water, the separated flocculate (sludge) is discharged into a sludge tank, the sludge is pumped to a screw stacking machine by a sludge pump to be dewatered, and dewatered sludge with low water content is separated out and is pulled by a truck for subsequent treatment. It should be noted that the sludge tank contains not only flocs obtained after the ultrafiltration treatment but also contaminants discharged from the electric desiliconization apparatus and precipitated contaminants generated in other processes.
And the salt water after the ultrafiltration treatment, namely the ultrafiltration treatment water is pressurized by a high-pressure pump and then enters an SRO reverse osmosis system for salt concentration, and in order to ensure the SRO reverse osmosis membrane to operate stably, in a preferred embodiment of the invention, a high-silicon scale inhibitor is added into the ultrafiltration treatment water before the reverse osmosis treatment. The high-silica scale inhibitor is optimized according to the characteristics of silica scale, preferably, the high-silica scale inhibitor is organic phosphate, the using amount of the high-silica scale inhibitor is 0.001-0.003kg/t of water, the high-silica scale inhibitor has high dispersibility, enhances the dispersion effect on soluble silicon, and is used for controlling scale formation and deposits in a reverse osmosis membrane separation system and reducing particle blockage.
The salt content of the concentrated water concentrated by the reverse osmosis system is about 12 percent, and the concentrated water is pumped to an evaporation system for evaporation treatment to obtain the industrial I class anhydrous sodium sulfate with more than first-class quality. The evaporation system can adopt multi-effect evaporation or MVR evaporation system. And sending the evaporation condensed water of the evaporation system and the 'clear water' concentrated by the reverse osmosis system to a clear water tank for a white carbon black production system to use. In the present invention, "concentrated water" refers to wastewater with high salt content generated in the reverse osmosis desalination process, and "clear water" refers to desalted water generated in the reverse osmosis desalination process.
The invention discloses a process method for treating precipitated white carbon black wastewater, which comprises the following steps of carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater through an electric desiliconization device; carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water; performing reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water; and sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate. Experiments prove that compared with the prior art, the process method disclosed by the invention can effectively remove soluble silicon in the precipitated white carbon black wastewater, well solves the problem of scaling and blocking of an ultrafiltration membrane and a reverse osmosis membrane, greatly prolongs the service time of the membrane, and realizes zero discharge of the precipitated white carbon black wastewater.
For further description of the scheme of the present application, experiments and verifications are performed on the process method for treating precipitated silica wastewater according to the present invention with reference to specific examples.
Example 1
Cooling precipitated white carbon black wastewater from a workshop wastewater tank through a wastewater cooling tower, sending the cooled wastewater to a precipitated wastewater tank for natural sedimentation, and neutralizing a small amount of alkali in the naturally sedimentated wastewater to be neutral and then carrying out electrolytic desiliconization through an electric desiliconization device. After electrolytic desiliconization, a small amount of desiliconization agent, coagulant aid and reducing agent are added, ultrafiltration treatment is carried out by an immersed ultrafiltration membrane component, and after a high-silicon scale inhibitor is added into ultrafiltration treatment water, reverse osmosis treatment is carried out by an SRO reverse osmosis system, so that clear water and concentrated water are obtained. Sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate. And sending the evaporation condensed water of the evaporation system and the clean water to a clean water tank for the white carbon black production system to use. Wherein the amounts of the respective chemicals are shown in table 2.
TABLE 2
Example 2
Cooling precipitated white carbon black wastewater from a workshop wastewater tank through a wastewater cooling tower, sending the cooled wastewater to a precipitated wastewater tank for natural sedimentation, adding a large amount of desiliconization agent, coagulant aid and reducing agent for chemical desiliconization, carrying out ultrafiltration treatment through an immersed ultrafiltration membrane component after chemical desiliconization, adding a high-silicon scale inhibitor into ultrafiltration treatment water, and then carrying out reverse osmosis treatment through an SRO reverse osmosis system to obtain 'clear water' and 'concentrated water'. Sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate. And sending the evaporation condensed water of the evaporation system and the clean water to a clean water tank for the white carbon black production system to use. Wherein the amounts of the respective chemicals are shown in Table 3
TABLE 3
Embodiment 1 is a process method for treating precipitated silica wastewater by using an electrolytic desiliconization technique, and embodiment 2 is different from embodiment 1 in that a conventional chemical desiliconization technique in the prior art is used before ultrafiltration treatment. Table 4 compares the silicon content data of the water before entering the reverse osmosis system for example 1 and example 2; table 5 shows the operating data for the reverse osmosis system of example 2; table 6 shows the operating data of the reverse osmosis system of example 1.
TABLE 4
TABLE 5
TABLE 6
As can be seen from Table 4, the conventional chemical silicon removal technology can only remove the silicon content in the silica white wastewater from 330mg/L to about 80mg/L, and although the service life of the membrane can be prolonged, the silicon blockage of the membrane can still be caused after the membrane is operated for a long time. As shown in Table 5, the flow rates of the clear water and the concentrated water in the operation process of the reverse osmosis membrane are reduced along with the time after the silicon is removed by adopting the traditional chemical agent, and the pressure difference between the inlet and the outlet of the reverse osmosis membrane is increased. This indicates that the reverse osmosis membrane becomes more clogged over time, and in fact after 97 hours of operation of the system, the reverse osmosis system is forced to shut down because of the clogging.
This is because the conventional chemical silicon removal technology has the following disadvantages:
1. the traditional chemical flocculation forms a flocculating agent with small specific surface area, low activity and more bound water, so the stability is poor and the separation is not facilitated; 2. in the traditional chemical flocculation, flocculates are suspended in liquid in the flocculation process, so that the removal of suspended matters is not facilitated; 3. traditional chemical flocculation cannot effectively remove tiny colloidal substances.
And the traditional chemical desiliconization treatment of precipitated silica wastewater has high cost and complex process. In the prior art, the oxidation, adsorption, flocculation, solid-liquid separation and other measures are generally carried out step by step, and the treatment process and the device are complicated and easily generate some uncontrollable adverse factors; a large amount of chemical agents are added in the chemical flocculation, secondary pollution is caused, and meanwhile, a process of neutralizing or removing anions is needed in the subsequent process, so that the process is complex; the total soluble solid content in the effluent of the chemical flocculation is higher, so that the water recovery cost is increased; the cost of the specific chemical agent is about 4.01 yuan/ton of wastewater, and the service life of the membrane is short and the membrane needs to be replaced frequently.
By utilizing the electrolytic silicon removal technology, the content of soluble silicon which is difficult to remove in the white carbon black wastewater can be economically removed from 330mg/L to below 30 mg/L. Practice proves that the silicon content of the ultrafiltration membrane and the reverse osmosis membrane is below 30mg/L and silicon blockage is not generated. And the water after silicon removal enters a relatively mature membrane separation concentration and evaporation system, so that the zero discharge of the purification treatment of the white carbon black wastewater can be realized. As shown in Table 6, the flow rates of the clear water and the concentrated water in the running process of the reverse osmosis membrane after the electrolytic silicon removal are not obviously changed along with the time, and the pressure difference between the inlet and the outlet of the reverse osmosis membrane is not changed, so that the reverse osmosis system can still normally run after continuously running for 384 hours, and the membrane blockage phenomenon cannot be generated. The electric desiliconization method adopted by the invention can achieve the purpose of removing silicon (mainly referring to soluble silicon) from the precipitated white carbon black wastewater by consuming electricity and a small amount of electrodes, the operation cost is relatively low, the electricity and electrode cost consumed by electric desiliconization is 1.4 yuan/ton of wastewater, and the increased cost is within the acceptable range of enterprises. Meanwhile, the service life of the membrane is longer, so that the treatment cost of the precipitated white carbon black wastewater is greatly reduced.
Compared with the prior art, the invention also has the following advantages:
1. the specific surface area of a flocculating body formed in the flocculation process is large, the activity is high, and the bound water is less, so that the stability is high, the separation is easy, and the sedimentation time is greatly shortened; 2. the total soluble solid content in the effluent after flocculation by the technology is lower, so that the water recovery cost can be greatly reduced; 3. the metal hydroxide obtained by electrolysis has strong destabilization effect on the polluted colloid, so the invention is very effective in removing tiny colloid substances, and can greatly reduce the risk of blocking a subsequent reverse osmosis system membrane; 4. the technology of the invention does not need to add a large amount of chemical agents, thereby avoiding secondary pollution, and the electrolyzed metal hydroxide can lead the wastewater to be alkalescent in the flocculation process, which is more beneficial to flocculation and precipitation, therefore, only a small amount of alkali is needed to be added in the early stage to neutralize the wastewater to be neutral, thereby reducing the alkali dosage; 5. the technology of the invention can generate micro bubbles in the flocculation process, and can carry flocculate to float to the surface of liquid, thereby leading the flocculate to be easier to remove; 6. the technology of the invention integrates various means such as oxidation, adsorption, flocculation, air flotation, solid-liquid separation and the like, so that the process flow is greatly shortened, the treatment device is simple and easy to operate, and the space of the device is greatly reduced.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present application, and not to limit the same; although the present application has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not necessarily depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.
Claims (5)
1. A process method for treating precipitated silica wastewater is characterized by comprising the following steps:
carrying out electrolytic desiliconization treatment on the pretreated precipitated white carbon black wastewater by using an electric desiliconization device;
carrying out ultrafiltration treatment on the wastewater subjected to electrolytic desiliconization through an immersed ultrafiltration membrane component to obtain ultrafiltration treated water;
carrying out reverse osmosis treatment on the ultrafiltration treated water through an SRO reverse osmosis system to obtain clear water and concentrated water;
sending the concentrated water to an evaporation system for evaporation treatment to obtain anhydrous sodium sulfate;
wherein the pretreatment specifically comprises the following steps:
cooling precipitated white carbon black wastewater from a workshop wastewater tank by a wastewater cooling tower;
sending the cooled wastewater to a wastewater sedimentation tank for natural sedimentation;
adding alkali into the naturally settled wastewater to neutralize the wastewater to be neutral;
wherein, before the ultrafiltration treatment, a desiliconization agent, a coagulant aid and a reducing agent are added into the wastewater after the electrolytic desiliconization;
the silicon removing agent is FeCl3The dosage is 0.01-0.1kg/t water; the coagulant aid is PAM, and the dosage is 0.001-0.005kg/t water; the reducing agent is ammonium bisulfite, and the dosage is 0.001-0.005kg/t water.
2. The method of claim 1, wherein the method further comprises:
adding a high silica scale inhibitor to the ultrafiltration treatment water prior to the reverse osmosis treatment.
3. The method of claim 2, wherein the high silica scale inhibitor is an organic phosphate salt and is used in an amount of 0.001 to 0.003kg/t water.
4. The method of claim 1, wherein the method further comprises:
and (4) conveying flocculate obtained after the ultrafiltration treatment to a sludge tank, and separating dewatered sludge by using a screw stacking machine.
5. The method of claim 1, wherein the method further comprises:
and sending the evaporation condensed water of the evaporation system and the clean water to a clean water tank for a white carbon black production system to use.
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