CN107899547A - A kind of waterworks dephosphorization adsorbent and preparation method thereof - Google Patents
A kind of waterworks dephosphorization adsorbent and preparation method thereof Download PDFInfo
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- CN107899547A CN107899547A CN201710999606.4A CN201710999606A CN107899547A CN 107899547 A CN107899547 A CN 107899547A CN 201710999606 A CN201710999606 A CN 201710999606A CN 107899547 A CN107899547 A CN 107899547A
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/288—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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved 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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of waterworks dephosphorization adsorbent and preparation method thereof, by gardens deadwood leaf, potassium carbonate, diatomite, iron chloride, chitosan, the raw materials such as citric acid are made, adsorbent of the present invention has moderate pore passage structure and abundant activated adoption site, a small amount of divalence and ferric ion are generated in rich-phosphorus water body to be precipitated with the phosphate radical generation ferric phosphate in water and ferrous phosphate, and it is incorporated in the sorbing material of diatomite cladding, recycled finally by superparamagnetism, the present invention can be used as the technical solution that waterworks processing is polluted by sudden phosphorus, ensure that water-supply plant effluent quality is up to standard, it is also cheap with processing cost, it is easy to operate, the advantages for the treatment of of wastes with processes of wastes against one another and non-secondary pollution.
Description
Technical field
The present invention relates to water-treatment technology field, more particularly to a kind of waterworks dephosphorization adsorbent and preparation method thereof.
Background technology
In recent years, because being influenced be subject to heavy rain, the problem of environmental pollution in sudden face source causes water head site water systems'phosphorus exceeded
It is more prominent.Some researches show that there are certain relation for the growth of phosphorus content and bacterium in drinking water.When ρ (P) is in 1-3 μ g/
During L, phosphorus becomes the restriction factor that microorganism grows in drinking water.The excessive microorganism easily triggered in drinking water of phosphorus content is once again
Breeding, is difficult to ensure that the biological stability of drinking water, so as to threaten the safety of drinking water in course of conveying.
In traditional handicraft, waterworks use chemical coagulation dephosphorization method there are it is of high cost, excess sludge is more, coagulation effect
It is unstable, introduce the shortcomings of other metal ions, and average removal rate is only 66%.Once the sudden phosphorus pollution of generation, conventional
Technique is difficult to ensure that drinking water safety.In recent years, modified turf and zeolite are included to the minimizing technology of phosphorus in Polluted raw water
Absorption method, modified apply Al sand and modified apply Fe sand method, activated carbon fibre biomembrane curtain method etc..But there are cost for these methods
Height, treatment effeciency is low, effect is unstable, starts the shortcomings of slow.Thus, it is necessary to researching and developing can quickly start and effectively remove originally
The new material of the sudden phosphorus pollution of water factory's water inlet.
Magnetic nano-particle is as a kind of new material developed in recent years, not only with nano effect, i.e. surface
Effect, small-size effect, macro quanta tunnel effect and bulk effect, also with magnetic property, such as superparamagnetism and high magnetization
The characteristics such as rate.Its application develops into high-technology field from traditional technical field, is expanded to from simple magnetics scope
With the relevant interdisciplinary field of magnetics.Among these ferroferric oxide magnetic nano-particles on the one hand because its have can be with biology
The special functional group of active material reaction, can be as the carrier of bioactive substance, on the other hand again because it is with superparamagnetic
Property, it under the action of externally-applied magnetic field, can quickly, simply separate, make it in wastewater treatment, exhaust-gas treatment, soil remediation, microwave
The research in the fields such as absorption becomes increasingly active, and shows preferable application prospect.
Since the size of nano-particle is very small, there is very high surface energy, be a kind of thermodynamic unstable system, easily
Larger particle is agglomerated into, and since nanoparticle surface carries many chemical bonds, there can be a very active chemical property, four
Fe 3 O magnetic nano-particle due to magnetic dipole gravitation between particle, is easily reunited as a kind of special nano-particle, is gathered
Synthesize offspring, be not easy to disperse, thus compared to general nano-particle for, the table of ferroferric oxide magnetic nano-particles
Face is modified just very necessary.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of waterworks dephosphorization adsorbent and its system
Preparation Method.
The present invention is achieved by the following technical solutions：
A kind of waterworks dephosphorization adsorbent, is prepared by the following method：
（1）It is sent into retort after dry, pulverize after gardens deadwood leaf is cleaned and is carbonized 40-50 minutes at 350-400 DEG C, is taken
Go out rear and potassium carbonate in mass ratio（3-4）：It is added to the water after 1 mixing and stirs and evenly mixs, when constant temperature oscillation 7-8 is small at 55-60 DEG C,
Filtering drying afterwards, is re-fed into high temperature furnace and activates, and takes out and is washed with water to pH neutrality after cooling, 100-120 is crushed after drying
Mesh sieve is spare；
（2）Iron chloride is pressed into solid-to-liquid ratio 1：（28-32）G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：（2.5-2.7）：
（0.7-0.8）, 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reaction kettle afterwards,
Be warming up to 200-220 DEG C, when reaction 5-6 is small after takes out and is cooled to room temperature, and with ethanol and clear water alternately cleaning removing impurity, by
Obtained solid is dried, and obtains Superparamagnetic Fe3O4 nanoparticles；
（3）Step 2 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in blender, and connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
Stirring 30-40 minutes, products therefrom ethanol and clear water are alternately cleaned, until pH is 7, be re-fed into drying box after stirring
In dried, it is spare that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding；
（4）By step 1 resulting material and step 3 gained nano-particle in mass ratio（5-6）：Quality point is added to after 1 mixing
Number is in the hydrochloric acid solution of 8-12%, when stirring 2-3 is small at 60-70 DEG C, centrifuges after cooling, is washed with clear water to no chlorion
In the presence of being dried for standby；
（5）By step 4 resulting material and diatomite in mass ratio 1：（1-2）It is granulated in mixing input comminutor, up to the present invention
Adsorbent.
The step 1 high temperature stove activation condition is to be activated 80-100 minutes at 800-840 DEG C.
Ultrasound condition is to be ultrasonically treated 10-12 minutes under 35-38kHz in the step 2.
Ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are in the step 3（5-6）：（1-1.2）：
（2-2.5）.
The application method of the waterworks dephosphorization adsorbent, phosphorus polluted-water quality 0.05-0.5% is pressed by adsorbent
Uniformly input polluted-water in, when 2-3 is small after pass through externally-applied magnetic field recycle adsorbent.
It is an advantage of the invention that：
The present invention prepares charcoal using garden waste and combines ferriferrous oxide nano-particle, makes absorption by acidification
Agent has moderate pore passage structure and abundant activated adoption site, improves the absorption property to phosphorus, wherein ferroso-ferric oxide
Nano-particle carries out surface modification so that chitosan and citric acid are compound to it, has been utilized respectively the electronegative polar end of citric acid and has borrowed
Help Coulomb force and ferroso-ferric oxide institute are positively charged to attract each other and the functional group in chitosan and its surface formation chemical bond
With reference to, thus to ferroso-ferric oxide particle surface locally coat, improve its inoxidizability, biocompatibility and in use
Dispersion stabilization, a small amount of divalence and ferric ion are generated in rich-phosphorus water body to generate ferric phosphate with the phosphate radical in water
Precipitate, and be incorporated in the sorbing material of diatomite cladding with ferrous phosphate, recycled finally by superparamagnetism, the present invention
The technical solution that waterworks processing is polluted by sudden phosphorus is can be used as, ensures that water-supply plant effluent quality is up to standard, also has
The advantages of processing cost is cheap, easy to operate, the treatment of wastes with processes of wastes against one another and non-secondary pollution.
Embodiment
A kind of waterworks dephosphorization adsorbent, is prepared by the following method：
（1）After dry, pulverize after gardens deadwood leaf is cleaned be sent into retort in carbonize 40 minutes at 350 DEG C, after taking-up and
Potassium carbonate in mass ratio 3.5：It is added to the water and stirs and evenly mixs after 1 mixing, when constant temperature oscillation 7 is small at 55 DEG C, filtering drying afterwards,
It is re-fed into high temperature furnace and is activated 80 minutes at 800 DEG C, takes out and be washed with water to pH neutrality after cooling, 100 mesh are crushed after drying
Sieve spare；
（2）Iron chloride is pressed into solid-to-liquid ratio 1：30g/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then add nothing thereto
Water sodium acetate and polyethylene glycol, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：2.6：0.8, it is warming up to 50
DEG C, it is stirred continuously to uniform mixed liquor is formed, is ultrasonically treated under 35kHz 10 minutes and is sent into after being uniformly dispersed in reaction kettle, risen
Temperature to 200 DEG C, when reaction 5 is small after takes out and is cooled to room temperature, and removing impurity is alternately cleaned with ethanol and clear water, by obtained solid
It is dry, obtain Superparamagnetic Fe3O4 nanoparticles；
（3）Step 2 gained ferriferrous oxide nano-particle is dispersed in 20% ethanol solution, then adds shell thereto and gathers
Sugar and citric acid, wherein ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are 5.5：1.2：2, mixed liquor is turned
Enter in blender, connection nitrogen protection, is warming up to 35 DEG C and is stirred 30 minutes with 800 revs/min, by products therefrom after stirring
Alternately cleaned with ethanol and clear water, until pH is 7, is re-fed into drying box and is dried, chitosan citrate is obtained after grinding
Duplex surface modification magnetic ferroferric oxide nano-particles are spare；
（4）By step 1 resulting material and step 3 gained nano-particle in mass ratio 5：Being added to mass fraction after 1 mixing is
In 8% hydrochloric acid solution, when stirring 2 is small at 60 DEG C, is centrifuged after cooling, washed to no chlorion and existed with clear water, drying is standby
With；
（5）By step 4 resulting material and diatomite in mass ratio 1：It is granulated in 1.5 mixing input comminutors, is inhaled up to the present invention
Attached dose.
Claims (5)
1. a kind of waterworks dephosphorization adsorbent, it is characterised in that be prepared by the following method：
（1）It is sent into retort after dry, pulverize after gardens deadwood leaf is cleaned and is carbonized 40-50 minutes at 350-400 DEG C, is taken
Go out rear and potassium carbonate in mass ratio（3-4）：It is added to the water after 1 mixing and stirs and evenly mixs, when constant temperature oscillation 7-8 is small at 55-60 DEG C,
Filtering drying afterwards, is re-fed into high temperature furnace and activates, and takes out and is washed with water to pH neutrality after cooling, 100-120 is crushed after drying
Mesh sieve is spare；
（2）Iron chloride is pressed into solid-to-liquid ratio 1：（28-32）G/mL is dissolved in ethylene glycol, is stirred continuously to being uniformly dissolved, then thereto
Anhydrous sodium acetate and polyethylene glycol are added, wherein iron chloride, anhydrous sodium acetate, the mass ratio of polyethylene glycol are 1：（2.5-2.7）：
（0.7-0.8）, 50-55 DEG C is warming up to, is stirred continuously to uniform mixed liquor is formed, ultrasonic disperse is uniformly sent into reaction kettle afterwards,
Be warming up to 200-220 DEG C, when reaction 5-6 is small after takes out and is cooled to room temperature, and with ethanol and clear water alternately cleaning removing impurity, by
Obtained solid is dried, and obtains Superparamagnetic Fe3O4 nanoparticles；
（3）Step 2 gained ferriferrous oxide nano-particle is dispersed in 20-25% ethanol solutions, then adds shell thereto
Glycan and citric acid, mixed liquor is transferred in blender, and connection nitrogen protection, is warming up to 35-40 DEG C and with 800-1000 revs/min
Stirring 30-40 minutes, products therefrom ethanol and clear water are alternately cleaned, until pH is 7, be re-fed into drying box after stirring
In dried, it is spare that chitosan-citric acid duplex surface modification magnetic ferroferric oxide nano-particles are obtained after grinding；
（4）By step 1 resulting material and step 3 gained nano-particle in mass ratio（5-6）：Quality point is added to after 1 mixing
Number is in the hydrochloric acid solution of 8-12%, when stirring 2-3 is small at 60-70 DEG C, centrifuges after cooling, is washed with clear water to no chlorion
In the presence of being dried for standby；
（5）By step 4 resulting material and diatomite in mass ratio 1：（1-2）It is granulated in mixing input comminutor, up to the present invention
Adsorbent.
2. the preparation method of waterworks dephosphorization adsorbent according to claim 1, it is characterised in that in the step 1
High temperature furnace activation condition is to be activated 80-100 minutes at 800-840 DEG C.
3. the preparation method of waterworks dephosphorization adsorbent according to claim 1, it is characterised in that in the step 2
Ultrasound condition is to be ultrasonically treated 10-12 minutes under 35-38kHz.
4. the preparation method of waterworks dephosphorization adsorbent according to claim 1, it is characterised in that in the step 3
Ferriferrous oxide nano-particle, chitosan, the mass ratio of citric acid are（5-6）：（1-1.2）：（2-2.5）.
5. the application method of claim 1-4 any one of them waterworks dephosphorization adsorbent, it is characterised in that by adsorbent
Uniformly put into by phosphorus polluted-water quality 0.05-0.5% in polluted-water, when 2-3 is small after pass through externally-applied magnetic field recycle adsorbent
Can.
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Cited By (5)
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| CN109173993A (en) * | 2018-09-18 | 2019-01-11 | 西安科技大学 | A kind of preparation method and application of magnetism straw charcoal |
| CN109225153A (en) * | 2018-10-22 | 2019-01-18 | 北京科技大学 | The preparation and its application method of the adsorbent material of trace amounts of phosphorus in a kind of removing water |
| CN109847721A (en) * | 2019-01-16 | 2019-06-07 | 南昌航空大学 | A kind of preparation method of the surface imprinted microballoon of superparamagnetism perfluoro octane sulfonate |
| CN112221466A (en) * | 2020-09-30 | 2021-01-15 | 中国地质大学（北京） | Phosphate-iron oxide modified biochar composite material, and preparation method and application thereof |
| CN113908652A (en) * | 2021-09-09 | 2022-01-11 | 济南市平阴县玛钢厂 | Process for reducing smoke dust emission of cupola furnace in foundry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109173993A (en) * | 2018-09-18 | 2019-01-11 | 西安科技大学 | A kind of preparation method and application of magnetism straw charcoal |
| CN109225153A (en) * | 2018-10-22 | 2019-01-18 | 北京科技大学 | The preparation and its application method of the adsorbent material of trace amounts of phosphorus in a kind of removing water |
| CN109225153B (en) * | 2018-10-22 | 2020-09-11 | 北京科技大学 | Preparation and application method of adsorbing material for removing trace phosphorus in water |
| CN109847721A (en) * | 2019-01-16 | 2019-06-07 | 南昌航空大学 | A kind of preparation method of the surface imprinted microballoon of superparamagnetism perfluoro octane sulfonate |
| CN112221466A (en) * | 2020-09-30 | 2021-01-15 | 中国地质大学（北京） | Phosphate-iron oxide modified biochar composite material, and preparation method and application thereof |
| CN113908652A (en) * | 2021-09-09 | 2022-01-11 | 济南市平阴县玛钢厂 | Process for reducing smoke dust emission of cupola furnace in foundry |
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Application publication date: 20180413 |