CN105502558B - A kind of preparation method of activated sludge and Nanoscale Iron carbon/carbon-copper composite material - Google Patents
A kind of preparation method of activated sludge and Nanoscale Iron carbon/carbon-copper composite material Download PDFInfo
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- CN105502558B CN105502558B CN201510916740.4A CN201510916740A CN105502558B CN 105502558 B CN105502558 B CN 105502558B CN 201510916740 A CN201510916740 A CN 201510916740A CN 105502558 B CN105502558 B CN 105502558B
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0233—Compounds of Cu, Ag, Au
- B01J20/0237—Compounds of Cu
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
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Abstract
The invention provides the preparation method of a kind of activated sludge and Nanoscale Iron carbon/carbon-copper composite material.The preparation method of this activated sludge and Nanoscale Iron carbon/carbon-copper composite material, comprises the following steps：1) pretreatment of activated sludge；2) preparation of liquid-phase reduction solution；3) preparation of composite；4) drying of composite.The present invention is prepared using activated sludge as carrier using sodium borohydride liquid phase reduction, and the composite organically combines activated sludge absorption performance and Nanoscale Iron strong reducing property, gives full play to the advantage of two kinds of materials.The iron copper binary metal system of formation, had both improved the aerial stability of Nanoscale Iron, increased the ironing surface activated adoption point of nanometer again, improved absorption and reducing property of the composite applied to treatment of Organic Wastewater.Wide using the particle size distribution range of activated sludge, surface area is big, and flco is in netted mechanism, is good carrier, and by activated sludge quilt, waste be changed into values, the treatment of wastes with processes of wastes against one another, has higher environmental benefit and economic benefit.
Description
Technical field
The invention belongs to field of material technology, is related to a kind of composite, particularly a kind of activated sludge and Nanoscale Iron copper
The preparation method of composite.
Background technology
Activated sludge is town domestic sewage treatment plant caused deposit during the dirty water decontamination handles, is that processing is dirty
The discarded object of solid-state, semisolid and liquid caused by water, its enormous amount, rapid development, it has also become a kind of new pollution sources,
Great threat is brought to urban environment, solves the problems, such as that activated sludge disposal is extremely urgent.Activated sludge contains 60%~70%
Thick protein, 25% or so carbohydrate, these organic components contain the carboxyl with absorption property, hydroxyl, amino, phosphorus
Acyl group and mercapto functional group, it is commonly used to manufacture adsorbent progress recycling.
Patent (application number：CN200910050238) " a kind of preparation method and applications of mud adsorbent ", patent (Shen
Please number：CN201210135162) " preparation method and applications of residual active sludge adsorbent " and patent (application number：
CN201510311930) patent such as " a kind of modified paper mill sludge adsorbent and preparation method and application " discloses various active
The preparation method of mud adsorbent.These methods add activator and presoma slurries are made, impregnate all using activated sludge as raw material
Dry, carbonize again afterwards.These methods come with some shortcomings：First, preparation technology flow is complicated, preparation time is long, cost is high；Two
Be single use activated sludge has certain limitation as adsorbent, its absorption property and effect, and activated sludge is inhaled
Pollutant is not destroyed or reduced to release toxin by attached pollutant.When this causes the adsorption capacity of activated sludge with using
Between extension and gradually reduce, be inevitably generated secondary pollution problem.Need to develop Mobyneb municipal sludge composite wood
Expect to improve its disposal ability.In recent years, during treatment of Organic Wastewater, Nanoscale Iron compares surface because its particle scale is small
Product is big, and reducing power is strong and receives much attention, but Nanoscale Iron is presented inactivation, reunites, reclaims the problems such as difficult in use,
Need to be loaded on carrier to strengthen practicality.
The content of the invention
The purpose of the present invention is above mentioned problem be present for existing technology, it is proposed that one kind is load using activated sludge
Body, prepared using sodium borohydride liquid phase reduction and have activated sludge absorption performance and Nanoscale Iron strong reducing property energy concurrently, improved compound
Materials application is in the activated sludge of the combination property for the treatment of of Organic Wastewater and the preparation method of Nanoscale Iron carbon/carbon-copper composite material.
The purpose of the present invention can be realized by following technical proposal：A kind of activated sludge and Nanoscale Iron carbon/carbon-copper composite material
Preparation method, comprise the following steps：
1) pretreatment of activated sludge：It will be crushed after the activated sludge drying of town domestic sewage treatment plant, sieving, use nitre
Acid soak, filter, clean up, it is standby after drying；
2) preparation of liquid-phase reduction solution：Iron chloride and copper chloride ultrasound are dissolved in 90% ethanol solution, in room temperature
Solution A is obtained after lower supersonic oscillations；The activated sludge that step 1) is obtained is mixed in three-neck flask with solution A, and magnetic force stirs
Mixture B is obtained after mixing；With deionized water dissolving sodium borohydride, solution C is obtained；
3) preparation of composite：Under the protective condition of nitrogen, the obtained solution C of step 2) is at the uniform velocity added dropwise to step 2)
In obtained mixture B, then it is sufficiently stirred, after solution C all drips off, then carries out magnetic agitation；
4) drying of composite：The composite that step 3) is obtained carries out rapid filtration under suction, is then placed in vacuum drying
It is dried to obtain the activated sludge and Nanoscale Iron carbon/carbon-copper composite material of solid-state in case.
In the preparation method of this activated sludge and Nanoscale Iron carbon/carbon-copper composite material, activated sludge is derived from town domestic sewage processing
The waste sludge of factory.The broken of activated sludge can use ball milling crusher machine, and obtain varigrained sludge by different screen clothes.
Suction filtration can use circulating water type vavuum pump pumping and filtering device.Supersonic oscillations can use ultrasonic oscillator.
In the preparation method of above-mentioned activated sludge and Nanoscale Iron carbon/carbon-copper composite material, in step 1), the activity is dirty
The drying temperature of mud is 105~120 DEG C, and drying time is 20~24h；Sludge granularity after the activated sludge is broken can be 60
~100 mesh；The nitric acid is 0.1~0.2mol/L salpeter solution, and adds 2~3mL salpeter solutions to soak by every gram of activated sludge
Steep 20~24h；Cleaning is washed rapidly to neutrality with deionized water, and the temperature of standby drying is 105~120 DEG C, its drying time
For 10~12h.
In the preparation method of above-mentioned activated sludge and Nanoscale Iron carbon/carbon-copper composite material, in step 2), the solution A
The mass ratio of iron chloride and copper chloride is 10：1~20：1, iron chloride and copper chloride and 90% ethanol solution quality and volume ratio
For 1g：10mL~1g：15mL；The duration of oscillation of ultrasonic wave is 30~40min；When activated sludge mixes with solution A, by every gram
Activated sludge adds 10~20mL solution A to mix after pretreatment；The time of magnetic agitation is 60~120min；In the solution C
The quality of sodium borohydride and deionized water and volume ratio are 1g：50mL~2g：50mL.
In the preparation method of above-mentioned activated sludge and Nanoscale Iron carbon/carbon-copper composite material, in step 3), the nitrogen
Flow velocity is 10~20mL/min；The drop rate of solution C is 1~2 drop/s, and the volume ratio of solution C and solution B is 1：1~1：2；
After solution C all drips off, the time of magnetic agitation is 30~40min.
It is described quickly to take out in step 4) in the preparation method of above-mentioned activated sludge and Nanoscale Iron carbon/carbon-copper composite material
The time of filter is 3~5min；The drying temperature of the vacuum drying chamber is 105~120 DEG C, and drying time can be 10~12h.
Compared with prior art, the preparation method of this activated sludge and Nanoscale Iron carbon/carbon-copper composite material is using activated sludge as load
Body, is prepared using sodium borohydride liquid phase reduction, and the composite has activated sludge absorption performance and Nanoscale Iron strong reducing property
Combine machine, give full play to the advantage of two kinds of materials.The iron copper binary metal system of formation, had both improved Nanoscale Iron in air
In stability, again increase the ironing surface activated adoption point of nanometer, improve composite be applied to treatment of Organic Wastewater suction
Echo reducing property.Because the particle size distribution range of the activated sludge of town domestic sewage treatment plant is wide, surface area is big, and flco is in
Netted mechanism, it is good carrier, the energy of adsorption of activated sludge can be improved by developing activated sludge and Nanoscale Iron carbon/carbon-copper composite material
Power, strengthen the strong reducing power of Nanoscale Iron again, while waste be changed into values by activated sludge quilt again, the treatment of wastes with processes of wastes against one another, has higher Environmental Effect
Benefit and economic benefit.It is trickle applied to particle present in organic wastewater instant invention overcomes current Nanoscale Iron, it is volatile in water
Living and cohesion, it is difficult to the shortcomings of reclaiming and reusing, in addition, this method technological process of production is short, the prices of raw materials are low, can be big
Amplitude reduction production cost.
Brief description of the drawings
Fig. 1 be embodiment one to three monomer and composite to benzole soln and the clearance form of phenol solution.
Fig. 2 is municipal sludge/Nanoscale Iron carbon/carbon-copper composite material XRD x ray diffration pattern xs of embodiment one to three.
Embodiment
It is the specific embodiment of the present invention and with reference to accompanying drawing below, technical scheme is further described,
But the present invention is not limited to these embodiments.
Embodiment one
Using the activated sludge of town domestic sewage treatment plant as carrier, it is dirty that activity is prepared using sodium borohydride liquid phase reduction
Mud and Nanoscale Iron carbon/carbon-copper composite material, specific implementation step are：
The activated sludge of town domestic sewage treatment plant is dried into 24h in 105 DEG C of baking oven, then crushed, crosses 60
Mesh sieve.
Activated sludge after sieving is filtered by every gram plus 2mL of 0.1mol/L salpeter solution immersion 24h and is used distilled water
Rapid washing is placed in 105 DEG C of baking oven after drying 10h, saved backup to neutrality.
10.0g iron chloride and 1.0g copper chloride ultrasounds are dissolved in 110mL 90% ethanol solution, at room temperature ultrasonic wave
Solution A is obtained after vibration 30min.Activated sludge is mixed in three-neck flask with solution A after 6.0g is pre-processed, magnetic agitation
120min obtains solution B.1g sodium borohydrides are taken to add 50mL deionized water dissolvings to obtain solution C in dropping funel.
The flow velocity for adjusting nitrogen is 15mL/min, after leading to nitrogen 5min, adjusts the piston in dropping funel, makes solution C with 1
Drop/s speed, it is added drop-wise in the mixture B at the uniform velocity stirred, it is whole that process control is added dropwise in 30min.Treat that solution C is all dripped
After complete, then magnetic agitation 30min.It is transferred to after the composite rapid filtration under suction of formation in culture dish, in 105 DEG C of vacuum drying
10h is dried in case, that is, obtains activated sludge and Nanoscale Iron carbon/carbon-copper composite material.
Embodiment two
The activated sludge of town domestic sewage treatment plant is dried into 20h in 120 DEG C of baking oven, then crushed, crosses 80
Mesh sieve.
Activated sludge after sieving is filtered and with distilling by every gram plus 2.5mL of 0.1mol/L salpeter solution immersion 20h
Washing to neutrality, is placed in 120 DEG C of baking oven after drying 10h, saved backup water rapidly.
7.5g iron chloride and 0.5g copper chloride ultrasounds are dissolved in 100mL 90% ethanol solution, at room temperature ultrasonic wave
Solution A is obtained after vibration 30min.Activated sludge is mixed in three-neck flask with solution A after 4.0g is pre-processed, magnetic agitation
90min obtains solution B.1g sodium borohydrides are taken to add 50mL deionized water dissolvings to obtain solution C in dropping funel.
The flow velocity for adjusting nitrogen be 10mL/min, after leading to nitrogen 10min, the piston in adjustment dropping funel, make solution C with
1 drop/s speed, it is added drop-wise in the mixture B at the uniform velocity stirred, it is whole that process control is added dropwise in 40min.Treat that solution C is all dripped
After complete, then magnetic agitation 30min.It is transferred to after the composite rapid filtration under suction of formation in culture dish, in 120 DEG C of vacuum drying
10h is dried in case, that is, obtains activated sludge and Nanoscale Iron carbon/carbon-copper composite material.
Embodiment three
The activated sludge of town domestic sewage treatment plant is dried into 22h in 110 DEG C of baking oven, then crushed, crosses 100
Mesh sieve.
Activated sludge after sieving is filtered and with distilling by every gram plus 3.0mL of 0.1mol/L salpeter solution immersion 24h
Washing to neutrality, is placed in 110 DEG C of baking oven after drying 12h, saved backup water rapidly.
10.0g iron chloride and 0.5g copper chloride ultrasounds are dissolved in 100mL 90% ethanol solution, at room temperature ultrasonic wave
Solution A is obtained after vibration 30min.Activated sludge is mixed in three-neck flask with solution A after 5.0g is pre-processed, magnetic agitation
60min obtains solution B.2g sodium borohydrides are taken to add 100mL deionized water dissolvings to obtain solution C in dropping funel.
The flow velocity for adjusting nitrogen is 20mL/min, after leading to nitrogen 5min, adjusts the piston in dropping funel, makes solution C with 2
Drop/s speed, it is added drop-wise in the mixture B at the uniform velocity stirred, it is whole that process control is added dropwise in 60min.Treat that solution C is all dripped
After complete, then magnetic agitation 30min.It is transferred to after the composite rapid filtration under suction of formation in culture dish, in 110 DEG C of vacuum drying
12h is dried in case, that is, obtains activated sludge and Nanoscale Iron carbon/carbon-copper composite material.
Weigh the preparation of three above embodiment activated sludge and Nanoscale Iron carbon/carbon-copper composite material with it is single pretreated
Activated sludge, Nanoscale Iron 0.1g are added in 250mL 10mg/L benzole soln and 20mg/L phenol solution successively, at room temperature
Magnetic agitation centrifuges after 1 hour, the benzene and phenol concentration of supernatant measure remaining is taken, as shown in figure 1, showing various embodiments above
The activated sludge and Nanoscale Iron carbon/carbon-copper composite material of preparation are respectively provided with good adsorption capacity and reducing property.
The XRD x ray diffration pattern xs of municipal sludge made from example one to three and Nanoscale Iron carbon/carbon-copper composite material are as shown in Figure 2：Should
For composite in 30 °~90 ° of 2 θ angles, there is obvious diffraction maximum at 44.75 ° in sample.Corresponding to body-centred cubic α-Fe
110 diffraction (d=0.202 7nm), while have also appeared and connect with body-centred cubic α-Fe 200 diffraction (d=0.202 7nm)
64.88 ° of near diffraction, the Nanoscale Iron for showing activated sludge load is mainly α-Fe, has stronger reproducibility.
Specific embodiment described herein is only to spirit explanation for example of the invention.Technology belonging to the present invention is led
The technical staff in domain can be made various modifications or supplement to described specific embodiment or be replaced using similar mode
Generation, but without departing from the spiritual of the present invention or surmount scope defined in appended claims.
Claims (3)
1. the preparation method of a kind of activated sludge and Nanoscale Iron carbon/carbon-copper composite material, it is characterised in that comprise the following steps：
1）The pretreatment of activated sludge：It will crush, sieving, soaked with nitric acid after the activated sludge drying of town domestic sewage treatment plant
Bubble, filter, clean up, it is standby after drying；The drying temperature of the activated sludge be 105~120 DEG C, drying time be 20~
24h；Sludge granularity after the activated sludge is broken can be 60~100 mesh；
The nitric acid is 0.1~0.2mol/L salpeter solution, and adds 2~3mL salpeter solutions to soak 20 by every gram of activated sludge
~24h；Cleaning is washed rapidly to neutrality with deionized water, and the temperature of standby drying is 105~120 DEG C, and its drying time is 10
~12h；
2）The preparation of liquid-phase reduction solution：Iron chloride and copper chloride ultrasound are dissolved in 90% ethanol solution, surpassed at room temperature
Solution A is obtained after sonication；By step 1）Obtained activated sludge is mixed in three-neck flask with solution A, after magnetic agitation
Obtain mixture B；With deionized water dissolving sodium borohydride, solution C is obtained；
The iron chloride of the solution A and the mass ratio of copper chloride are 10：1~20：1, iron chloride and copper chloride and 90% ethanol
Solution quality and volume ratio are 1g：10mL~1g：15mL；The duration of oscillation of ultrasonic wave is 30~40min；Activated sludge with it is molten
When liquid A is mixed, 10~20mL solution A is added to mix by activated sludge after every gram of pretreatment；The time of magnetic agitation is 60~120
min；The quality of sodium borohydride and deionized water and volume ratio are 1g in the solution C：50mL~2g：50mL；
3）The preparation of composite：Under the protective condition of nitrogen, step 2 is at the uniform velocity added dropwise）Obtained solution C is to step 2）Obtain
Mixture B in, be then sufficiently stirred, after solution C all drips off, then carry out magnetic agitation；
4）The drying of composite：By step 3）Obtained composite carries out rapid filtration under suction, is then placed in vacuum drying chamber
It is dried to obtain the activated sludge and Nanoscale Iron carbon/carbon-copper composite material of solid-state.
2. preparation method according to claim 1, it is characterised in that in step 3）In, the flow velocity of the nitrogen for 10~
20 mL/min；The drop rate of solution C is 1~2 drop/s, and the volume ratio of solution C and solution B is 1：1~1：2；Treat that solution C is complete
After portion drips off, the time of magnetic agitation is 30~40min.
3. preparation method according to claim 1, it is characterised in that in step 4）In, the time of the rapid filtration under suction is 3
~5 min；The drying temperature of the vacuum drying chamber is 105~120 DEG C, and drying time can be 10~12h.
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| CN107915377B (en) * | 2017-12-12 | 2020-11-10 | 陕西祥宇环保科技有限公司 | Urban domestic sewage treatment method |
| CN109485216A (en) * | 2018-12-27 | 2019-03-19 | 闽南师范大学 | A kind of preparation method of autumn eggplant plumular axis extracting solution synthesizing activity sludge cuprous oxide composite material |
| CN110508242A (en) * | 2019-06-12 | 2019-11-29 | 董良杰 | A kind of biology ceramic composite material and its bagged product, preparation method and application |
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| CN102259032B (en) * | 2011-05-31 | 2013-07-24 | 厦门大学嘉庚学院 | Method for preparing activated sludge / titanium dioxide composite material |
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