CN103011535A - Hydro-thermal treatment method for electroplating sludge - Google Patents
Hydro-thermal treatment method for electroplating sludge Download PDFInfo
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- CN103011535A CN103011535A CN2012101174707A CN201210117470A CN103011535A CN 103011535 A CN103011535 A CN 103011535A CN 2012101174707 A CN2012101174707 A CN 2012101174707A CN 201210117470 A CN201210117470 A CN 201210117470A CN 103011535 A CN103011535 A CN 103011535A
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Abstract
The invention discloses a hydro-thermal treatment method for electroplating sludge, which comprises the following steps of: firstly mixing electroplating sludge with water so as to form electroplating sludge fluid; feeding the electroplating sludge fluid into a continuous high-temperature and high-pressure reaction kettle, and after a fixed volume is achieved, stopping feeding; raising the internal temperature of the kettle so as to carry out hydro-thermal treatment; after the hydro-thermal treatment is completed, discharging heavy metal sludge hydro-thermal residues subjected to reaction, and carrying out filter pressing on the discharged heavy metal sludge hydro-thermal residues so as to obtain solid-phase hydro-thermal residues and liquid-phase hydro-thermal water; carrying out immersion cleaning on the solid-phase hydro-thermal residues by using a sulfuric acid and carrying out filter pressing on the solid-phase hydro-thermal residues so as to obtain acid-washing liquor and hydro-thermal residue precipitates, and drying and grinding the hydro-thermal residue precipitates subjected to each acid-washing process; and uniformly mixing the acid-washing liquor and the liquid-phase hydro-thermal water obtained each time, and then preparing ferrite by using a chemical co-precipitation method. According to the hydro-thermal treatment method disclosed by the invention, the leaching of heavy metals can be efficiently realized, and the heavy metals can be subjected to effective separation and recycling by taking subsequent separation measures. The moisture content of sludge can be greatly reduced through a plate-and-frame filter press, so that the volume of the sludge residues is reduced, the heavy metal dissolution rate of the residues is greatly reduced, and the form is more stable.
Description
Technical field
The present invention relates to industrial waste liquid waste disposal and resource recycling and environmental protection and energy saving technical field, particularly a kind of electroplating sludge hydro-thermal treatment method.
Background technology
Mud is the solid precipitation material that is produced by sewage treatment process.In solid waste pollution harm, the most serious is the pollution of Hazardous wastes, so the improvement emphasis of solid waste is the improvement of hazardous solid waste, is a class in the hazardous solid waste and contain the heavy metal water treatment sludge.Electroplating sludge is electroplating industry wastewater treatment " final state thing ", and the noble metals such as a large amount of copper, nickel, chromium, iron, zinc are contained in the inside.Electroplating sludge is mainly derived from the various electroplating effluents of industrial Electroplate Factory and cell liquid is processed the rear solid waste that produces by liquid phase chemical, because it is different that each electroplates production technique and the treatment process of producer, the chemical composition very complex of electroplating sludge mainly contains heavy metal compound and the solubility salts such as chromium, iron, nickel, copper, zinc.
According to China Environmental Science Research Institute's measuring and calculating, by 2010, the wet mud that each municipal sewage plant of China produces will reach more than 3,000 ten thousand tons, account for more than 5% of China's year total solids waste discharge amount.Landfill, the transudate in the waste pit gentle cognition welding, polluted air and water source.Objectionable impurities enters Water table meeting polluted underground water environment in the transudate; The gases methane that landfill yard produces does not take appropriate measures and can set off an explosion; In addition, the place that is fit to Sludge landfill is also more and more limited because of a large amount of output of municipal sludge, the U.S. has closed a large amount of landfill yards in recent decades, and EU countries's landfill disposal in 1992 accounts for 40%, reduced to 17% in 2005, and the material of regulation institute landfill only limits to organic content＜50g/kg.Its calorific value of burning and processing sludge general requirement is more than 1000kJ/kg.The gases such as the Dioxins that produces during burning cause topsoil, and Heavy Metals in Sludge also spreads with flue dust.In addition, burning cost is 2～4 times of other treatment process.The technical costss such as the sludge dehydrating and drying of developing in the market, dosing curing are all at 80-100 unit/t, but sludge reduction and innoxious not thorough all still needs further to carry out landfill or burning disposal.
In recent years; promotion for purpose and the economic interests of protection of the environment; emerge large quantities of application emerging technologies and process the research of heavy metal sewage sludge, mainly contain chemical method, ion exchange method, activated carbon method, electrolytic process, evaporation concentration method, reverse osmosis method, osmosis method etc.It is reported that the Electroplate Factory of China about 41% adopts Chemical Method for Waste Water of Electroplate, in Japan, account for 85% with what chemical process was processed electroplating wastewater.Although chemical Treatment electroplated heavy metals waste water less investment, technology maturation, strong adaptability, level of automation are high, and along with the use of pH-ORP auto-controller, the chemical Treatment heavy metal wastewater thereby will have the trend of increase.But the disadvantage of chemical method is to produce a large amount of heavy metal sewage sludges, these mud contain the harmful heavy metal of hard degradation, it has the characteristics such as easy accumulation, unstable, easy loss, as not dealt carefully with, stack arbitrarily, then will cause serious secondary pollution, human body and ecotope will be impacted.
Chinese patent CN201010541598.7 has illustrated a kind of recycling processing method of heavy metal sewage sludge, it is that 30wt%～50wt% acid solution leaches the heavy metal in the sludge containing heavy metal with weight percent concentration first, be 14KHz～28KHz ultrasonication pickling liquor with frequency again, behind ultrasonic separation 30～60min, solid-liquid separation goes out the throw out of sulfur acid calcium and contains the acid solution of heavy metal ion, the acid solution that leaches is processed and is regulated after the pH value is 9 through ferrous sulfate, after adding the ferroxidant oxidation, form ferrite.The calcium sulfate precipitation thing forms gypsum after washing and drying.This invention is fit to process the various mud that contain heavy metal ion, and not only the technique versatility is good, and processing condition are simple; workable; more can accomplish scale production, be a kind for the treatment of of wastes with processes of wastes against one another, the treatment technology of energy-saving and emission-reduction, innoxious and resource regeneration sludge containing heavy metal.
Chinese patent CN201010242352.X relates to a kind for the treatment of agent and treatment process that contains electroplating sludge, specifically disclose a kind of heavy metal pollution bottle sediment curing agent, this solidifying agent comprises cement and flyash, and the mass ratio of flyash and cement is 1: (0.5～11).The curing of this solidifying agent may further comprise the steps: directly add the solidifying agent of this invention in electroplate to pollute, the consumption of solidifying agent is for electroplating 0.4～1.5 times of polluted bed mud quality, and the mixture maintenance 3d at least with adding behind the solidifying agent finishes solidification process.Solidifying agent of the present invention and curing not only processing cost are low, and solidification effect is desirable.
Chinese patent CN201010570514.2 relates to a kind of production technique for reducing content of heavy metals in municipal domestic sludge, the method is processed municipal sludge and is realized that health is innoxious by a thermophilic fermentation, and the physicochemical character of reformative sludge, make it to be fit to plant growth, then, plant the crop that has the heavy metal element accumulation ability that exceeds standard at mud, the heavy metal of mud is transferred in the plant, Of Heavy Metal Level In Sludge is significantly reduced, until reach the quality standard of organic fertilizer, then the raw materials for production as fertilizer utilize, and have positive effect to promoting solution domestic sludge soil, city to recycle safely.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of electroplating sludge hydro-thermal treatment method is provided, to realize changing waste into resources, change Hazardous wastes into general waste, so that follow-up further processing.
The objective of the invention is to be achieved through the following technical solutions:
The electroplating sludge hydro-thermal treatment method is first electroplating sludge to be mixed with 0.2～0.5 times of volume water, forms the electroplating sludge fluid; With fresh feed pump described electroplating sludge fluid is squeezed into the serialization high-temperature high-pressure reaction kettle again, stop charging after reaching fixing capacity; Open the heat riser of serialization high-temperature high-pressure reaction kettle, temperature in the serialization high-temperature high-pressure reaction kettle is increased to 200～300 ℃, pressure is that 5～8MPa carried out hydrothermal treatment consists 1～10 minute; After hydrothermal treatment consists is complete, open tapping channel, discharge reacted heavy metal sewage sludge hydro-thermal slag, meanwhile open fresh feed pump described electroplating sludge fluid is squeezed into the serialization high-temperature high-pressure reaction kettle to fixed capacity; The heavy metal sewage sludge hydro-thermal slag of discharging obtains solid phase hydro-thermal slag and liquid phase water hot water after press filtration; Solid phase hydro-thermal slag is that 20% sulfuric acid embathes 1～3 time according to the standard weight percent concentration of 150mL/100g, press filtration obtains pickle solution and hydro-thermal slag precipitation after each pickling, the hydro-thermal slag that merges after each time pickling is deposited in 105 ± 2 ℃ of lower oven dry, grind, be sieved into particle diameter less than the particle of 3mm, pack stand-by; Utilize chemical coprecipitation to make ferrite after merging each time pickle solution and liquid phase water hot water evenly mixing.
In a preferred embodiment of the invention, described press filtration adopts plate-and-frame filter press to carry out.
In a preferred embodiment of the invention, described serialization high-temperature high-pressure reaction kettle is the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle that the prosperous Tai Huagongshebeichang in Weihai produces.
In a preferred embodiment of the invention, heavy metal sewage sludge hydro-thermal slag and the electroplating sludge fluid of discharge carry out heat exchange by an interchanger, with preheating electroplating sludge fluid; Heavy metal sewage sludge hydro-thermal slag press filtration after condensation after the heat exchange obtains solid phase hydro-thermal slag and liquid phase water hot water.
Owing to adopted technical scheme as above, the present invention squeezes into effect that serialization high-temperature high-pressure reaction kettle to fixed capacity reach continuous and automatic thereby meanwhile open fresh feed pump with described electroplating sludge fluid discharging reacted heavy metal sewage sludge hydro-thermal slag.
The heavy metal sewage sludge hydro-thermal slag process press filtration that the present invention row states is water cut greatly, the volume of reduce mud residue, and residue leaching ability of heavy metal rate greatly reduces, and form is also more stable.The heavy metal that adheres to is extracted and isolates in the further pickling of solid phase hydro-thermal slag after the press filtration, reaches the effect of recycling.
Hydro-thermal treatment method of the present invention at 200～300 ℃, under the condition of 5～8MPa, makes the viscosity hydrolysis of organic matter in the mud by with the mud heating, destroys the colloidal structure of mud, can improve dewatering and anaerobic digestion performance simultaneously.With the increase of hydrothermal temperature and pressure, the particle collision probability increases, and intergranular collision has caused the destruction of colloidal structure, and irreducible water is separated with solid particulate.In addition, heating is decomposed the protein in the mud, and cell breaks, and the moisture in the born of the same parents is released.The mud of process hydrothermal treatment consists is in the situation of not adding flocculation agent, and mechanical dehydration can make the water ratio decrease.With this understanding, because mud forms, the change of structure, also greatly the reducing in conjunction with tightness degree of heavy metal element and colloid, organic substance and mud granule, thus enter in a large number in the hydro-thermal water.
Subcritical water thermal hydrolysis reaction of the present invention is green environmental protection technique, utilize hydro-thermal reaction that the larger molecular organics in the mud (such as protein etc.) is converted to low molecule organic matter at short notice (such as glucose, amino acid etc.), thus greatly improve the dehydrating effect of high water content sludge.
The present invention compares with additive method has following features:
(1) organic pollutant is innoxious, minimizing is thorough fast;
(2) the thorough water ratio of hydro-thermal reaction can be reduced to approximately 20%, has greatly improved the minimizing efficient of mud;
(3) heavy metal is through high temperature high pressure process, and salinity is high, residue leaching ability of heavy metal rate greatly reduces;
(4) since the hydro-thermal operating temperature far below burning method (more than 850 ℃), cost of erection and running cost be far below burning method, and can further reduce energy consumption by thermal exchange;
(5) processing speed is fast, capacity usage ratio is high, the operation operation is convenient, easily expand the scale of production etc.
Description of drawings
Fig. 1 is the schema of electroplating sludge hydro-thermal treatment method of the present invention.
Fig. 2 is the hydro-thermal increasing temperature and pressure graph of a relation of electroplating sludge hydro-thermal treatment method of the present invention.
Fig. 3 is hydro-thermal figure pressure rising time of electroplating sludge hydro-thermal treatment method of the present invention.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.
Put into modified tank after the unloading of mud car, add about 0.2 times of volume aqueous solution dilution, fluid state to be formed, be transported to hopper with worm conveyor, squeeze into the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle that the prosperous Tai Huagongshebeichang in Weihai produces through High pressure feeding pump again, stop charging after reaching fixing capacity.Open the heat riser of the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai, heating boosts to 5.33MPa, 232 ℃, the loading and unloading material valve of namely opening the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai enters remaining tank, about residence time 8min, opening lower discharge valve relies on the pressure pulse spoil disposal to basin, heavy metal sewage sludge hydro-thermal slag and the electroplating sludge fluid of discharging carry out heat exchange by an interchanger, with preheating electroplating sludge fluid.
Again through the plate-and-frame filter press press filtration, solid-liquid separation obtains solid phase hydro-thermal slag and liquid phase water hot water after the heavy metal sewage sludge hydro-thermal slag condensation after the heat exchange.Solid phase hydro-thermal slag is that 20% sulfuric acid embathes 1～3 time according to the standard weight percent concentration of 150mL/100g, press filtration obtains pickle solution and hydro-thermal slag precipitation after each pickling, the hydro-thermal slag that merges after each time pickling is deposited in 105 ± 2 ℃ of lower oven dry, grind, be sieved into particle diameter less than the particle of 3mm, pack stand-by.Utilize chemical coprecipitation to make ferrite after merging each time pickle solution and liquid phase water hot water evenly mixing.
Solid phase hydro-thermal slag is cleared up: take by weighing and dry the sample 1.000g that ground, be put in the polytetrafluoroethylene beaker, it is moistening to add a little deionized water, then adds 15mLHNO
3, slow thermal degradation on electrothermal oven adds glass cover to reflux, and steams near dried.Take off beaker, slightly cold rear adding nitration mixture (V (HNO
3): v (HClO
4)=1: 4) 10mL is put in and makes sample continuation decomposition on the electric furnace, steams near dried.Repeatedly add 10mLHNO after slightly cold
3, being evaporated near doing, sample steams to nearly canescence.Take off beaker, add 10% HNO
3Filter after the solution dissolving, constant volume is to be measured in the volumetric flask of 50mL.Learn through the ICP-AES detection: the clearance of Ni, Cu, Zn is as shown in table 1.
Table 1
Put into modified tank after the unloading of mud car, add about 0.2 times of volume aqueous solution dilution, fluid state to be formed, be transported to hopper with worm conveyor, squeeze into the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle that the prosperous Tai Huagongshebeichang in Weihai produces through High pressure feeding pump again, stop charging after reaching fixing capacity.Open the heat riser of the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai, heating boosts to 7.67MPa, 241 ℃, the loading and unloading material valve of namely opening the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai enters remaining tank, about residence time 8min, opening lower discharge valve relies on the pressure pulse spoil disposal to basin, heavy metal sewage sludge hydro-thermal slag and the electroplating sludge fluid of discharging carry out heat exchange by an interchanger, with preheating electroplating sludge fluid.
Again through the plate-and-frame filter press press filtration, solid-liquid separation obtains solid phase hydro-thermal slag and liquid phase water hot water after the heavy metal sewage sludge hydro-thermal slag condensation after the heat exchange.Solid phase hydro-thermal slag is that 20% sulfuric acid embathes 1～3 time according to the standard weight percent concentration of 150mL/100g, press filtration obtains pickle solution and hydro-thermal slag precipitation after each pickling, the hydro-thermal slag that merges after each time pickling is deposited in 105 ± 2 ℃ of lower oven dry, grind, be sieved into particle diameter less than the particle of 3mm, pack stand-by.Utilize chemical coprecipitation to make ferrite after merging each time pickle solution and liquid phase water hot water evenly mixing.
Hydro-thermal slag precipitation is cleared up: take by weighing and dry the sample 1.000g that ground, be put in the polytetrafluoroethylene beaker, it is moistening to add a little deionized water, then adds 15mLHNO
3, slow thermal degradation on electrothermal oven adds glass cover to reflux, and steams near dried.Take off beaker, slightly cold rear adding nitration mixture (V (HNO
3): v (HClO
4)=1: 4) 10mL is put in and makes sample continuation decomposition on the electric furnace, steams near dried.Repeatedly add 10mLHNO after slightly cold
3, being evaporated near doing, sample steams to nearly canescence.Take off beaker, add 10% HNO
3Filter after the solution dissolving, constant volume is to be measured in the volumetric flask of 50mL.Learn through the ICP-AES detection: the clearance of Ni, Cu, Zn is as shown in table 2.
Table 2
Put into modified tank after the unloading of mud car, add about 0.2 times of volume aqueous solution dilution, fluid state to be formed, be transported to hopper with worm conveyor, squeeze into the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle that the prosperous Tai Huagongshebeichang in Weihai produces through High pressure feeding pump again, stop charging after reaching fixing capacity.Open the heat riser of the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai, heating boosts to 7.98MPa, 256 ℃, the loading and unloading material valve of namely opening the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle of the prosperous Tai Huagongshebeichang production in Weihai enters remaining tank, about residence time 8min, opening lower discharge valve relies on the pressure pulse spoil disposal to basin, heavy metal sewage sludge hydro-thermal slag and the electroplating sludge fluid of discharging carry out heat exchange by an interchanger, with preheating electroplating sludge fluid.
Heavy metal sewage sludge hydro-thermal slag condensation after the heat exchange is again through filter press, and solid-liquid separation obtains solid phase hydro-thermal slag and liquid phase water hot water.Solid phase hydro-thermal slag is that 20% sulfuric acid embathes 1～3 time according to the standard weight percent concentration of 150mL/100g, press filtration obtains pickle solution and hydro-thermal slag precipitation after each pickling, the hydro-thermal slag that merges after each time pickling is deposited in 105 ± 2 ℃ of lower oven dry, grind, be sieved into particle diameter less than the particle of 3mm, pack stand-by.Utilize chemical coprecipitation to make ferrite after merging each time pickle solution and liquid phase water hot water evenly mixing.
Hydro-thermal slag precipitation is cleared up: take by weighing and dry the sample 1.000g that ground, be put in the polytetrafluoroethylene beaker, it is moistening to add a little deionized water, then adds 15mLHNO
3, slow thermal degradation on electrothermal oven adds glass cover to reflux, and steams near dried.Take off beaker, slightly cold rear adding nitration mixture (V (HNO
3): v (HClO
4)=1: 4) 10mL is put in and makes sample continuation decomposition on the electric furnace, steams near dried.Repeatedly add 10mLHNO after slightly cold
3, being evaporated near doing, sample steams to nearly canescence.Take off beaker, add 10% HNO
3Filter after the solution dissolving, constant volume is to be measured in the volumetric flask of 50mL.Learn through the ICP-AES detection: the clearance of Ni, Cu, Zn is as shown in table 3.
Table 3
Claims (4)
1. the electroplating sludge hydro-thermal treatment method is characterized in that first electroplating sludge being mixed with 0.2～0.5 times of volume water, forms the electroplating sludge fluid; With fresh feed pump described electroplating sludge fluid is squeezed into the serialization high-temperature high-pressure reaction kettle again, stop charging after reaching fixing capacity; Open the heat riser of serialization high-temperature high-pressure reaction kettle, temperature in the serialization high-temperature high-pressure reaction kettle is increased to 200～300 ℃, pressure is that 5～8MPa carried out hydrothermal treatment consists 1～10 minute; After hydrothermal treatment consists is complete, open tapping channel, discharge reacted heavy metal sewage sludge hydro-thermal slag, meanwhile open fresh feed pump described electroplating sludge fluid is squeezed into the serialization high-temperature high-pressure reaction kettle to fixed capacity; The heavy metal sewage sludge hydro-thermal slag of discharging obtains solid phase hydro-thermal slag and liquid phase water hot water after press filtration; Solid phase hydro-thermal slag is that 20% sulfuric acid embathes 1～3 time according to the standard weight percent concentration of 150mL/100g, press filtration obtains pickle solution and hydro-thermal slag precipitation after each pickling, the hydro-thermal slag that merges after each time pickling is deposited in 105 ± 2 ℃ of lower oven dry, grind, be sieved into particle diameter less than the particle of 3mm, pack stand-by; Utilize chemical coprecipitation to make ferrite after merging each time pickle solution and liquid phase water hot water evenly mixing.
2. electroplating sludge hydro-thermal treatment method as claimed in claim 1 is characterized in that described press filtration employing plate-and-frame filter press carries out.
3. electroplating sludge hydro-thermal treatment method as claimed in claim 1 is characterized in that described serialization high-temperature high-pressure reaction kettle is the GSHA-1 type permanent magnetism rotary stirring high-pressure kettle that the prosperous Tai Huagongshebeichang in Weihai produces.
4. electroplating sludge hydro-thermal treatment method as claimed in claim 1 is characterized in that heavy metal sewage sludge hydro-thermal slag and the electroplating sludge fluid of discharging carry out heat exchange by an interchanger, with preheating electroplating sludge fluid; Heavy metal sewage sludge hydro-thermal slag press filtration after condensation after the heat exchange obtains solid phase hydro-thermal slag and liquid phase water hot water.
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| CN107010806A (en) * | 2017-03-14 | 2017-08-04 | 北京顺鸿金建环境科技发展有限公司 | A kind of method that hydrothermal carbonization handles sludge |
| CN110523309A (en) * | 2019-10-14 | 2019-12-03 | 中煤科工清洁能源股份有限公司 | A method of the sedimentation method of modifying of waste, reforming system and high concentration slurry is prepared using modified product |
| CN111254285A (en) * | 2020-01-21 | 2020-06-09 | 东北师范大学 | Resource utilization method of electroplating waste mud |
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| CN111254285A (en) * | 2020-01-21 | 2020-06-09 | 东北师范大学 | Resource utilization method of electroplating waste mud |
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