CN106669606B - A kind of adsorption sustained-release filler and preparation method thereof for artificial swamp - Google Patents
A kind of adsorption sustained-release filler and preparation method thereof for artificial swamp Download PDFInfo
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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
- B01J20/12—Naturally occurring clays or bleaching 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
- B01J20/02—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
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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
- B01J20/20—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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/32—Biological treatment of water, waste water, or sewage characterised by the animals or plants used, e.g. algae
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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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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Abstract
The invention belongs to environmental friendly material fields, and in particular to a kind of adsorption sustained-release filler and preparation method thereof for artificial swamp.The preparation method of the filler successively include to the activation of the acid soak of basis material, to the polyaniline overlay film of basis material after activation, impregnate combined processing to the copper solution of basis material coated with film and handled with the mixed calcination pore-forming of biological material and adhesive.Large amount of adsorption, the adsorption capacity of adsorption sustained-release filler provided by the invention are strong, when in water inlet the pollutants such as nitrogen phosphorus because content is more can not be complete by the plant absorption on artificial swamp surface layer when, filler can effectively adsorb the pollutant having more；It also has slow-release capability, can be with nutriments such as slow release nitrogen and phosphorus, to meet the growth demand of plant when being unable to satisfy plant growth when the pollutant loads such as nitrogen phosphorus are low.The primary raw material for preparing the adsorption sustained-release material is that cheap products, the production costs such as montmorillonite, kaolin and attapulgite and biological material are low.
Description
Technical field
The invention belongs to environmental friendly material fields, and in particular to a kind of adsorption sustained-release filler and its system for artificial swamp
Preparation Method.
Background technique
In recent years, China's water environment situation deteriorates increasingly, occur lake eutrophication, immediate offshore area red tide, river and
The problems such as organic contamination of reservoir, threatens the diversion safety of resident and the health of the people.Wastewater treatment work
Skill is since it is good with effects of purification quality, capital construction operating cost is low, low energy consumption, maintenance management is simple, capacity of resisting impact load
The features such as strong, and can be provided for wild animal habitat, improve ecoscape aesthetic values, so sanitary sewage,
Industrial wastewater, agricultural area source sewage, urban storm runoff and eutrophication water etc. are widely used
Artificial swamp can be settled and can using in the root of water plant prosperity and filler particles interception sewage at present
Flocculated solid, while degrading by the microorganism for being attached to plant root to the harmful substance in sewage, reach water quality
The purpose of purification.Existing Artificial Wetland Techniques are disadvantageous in that, when water quality and quantity has large change or water plant
When the season of withered harvesting, the water outlet through artificial swamp may just be unable to satisfy requirement up to standard.
Summary of the invention
In order to overcome the shortcomings in the prior art, the present invention provide a kind of adsorption sustained-release filler that can be used for artificial swamp and its
Preparation method is laid with one layer of adsorption sustained-release filler in the packing layer of existing artificial swamp, the pollution when water body flows through, in water
Object a part is absorbed and used by plants, and a part is adsorbed by the adsorption sustained-release material, when the material concentrations such as nitrogen phosphorus are smaller in water inlet
When being unable to satisfy demand of plant growth, the organic matter and nitrogen phosphorus that filler slow release has been adsorbed in it grow needs for plant,
When the material concentrations such as nitrogen phosphorus are larger in water inlet, when plant can not be adsorbed completely, the absorption property of adsorbent material can use to dirt
Extra pollutant is adsorbed in water, so that water outlet meets requirement up to standard.
The technical scheme to solve the above technical problems is that a kind of adsorption sustained-release filler for artificial swamp
Preparation method comprising following steps:
S1. it activates: will be soaked in the basis material investment reactor after the screening of 200~2000 meshes and with acid solution
Not yet, stir-activating 1-12h is centrifugated and is washed to neutrality, dry to get activated matrix material, spare；
S2. overlay film: the activated matrix material in S1 is mixed with water, is beaten to obtain slurries, and acid solution is added, sequentially adds
Aniline and initiator, initiator are one of persulfates such as sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate or a variety of, can
Cause aniline polymerization reaction occurs and is sufficiently mixed with basis material, stirring at normal temperature reacts 2-8h, filters, washes, is dry, grinding
Mill, sieving, obtain 200~2000 mesh overlay film basis materials；
S3. compound: by the overlay film basis material in S2 and to contain Cu2+Solution mixing, extremely with the pH of buffer solution regulation system
Cu is washed with deionized into filtrate in isothermal reaction 0.5-4h at 6,40-80 DEG C, filtering, filter cake2+< 0.05mg/L, it is dry, it grinds
Mill obtains powdered containing carbon/carbon-copper composite material；
S4. it is calcined: in parts by weight, carbon/carbon-copper composite material, 10-20 parts of powdered biologicals will be contained in 60-80 parts of S3
Material (partial size is less than 200 mesh), 5-10 parts of adhesives and 10-20 parts of water are uniformly mixed, and are then forged at 150-400 DEG C
2-4h is burnt, is cooled to room temperature under oxygen-free environment to get the adsorption sustained-release filler for artificial swamp.
Specifically, basis material in S1 be in montmorillonite, kaolin and attapulgite any one or it is any a variety of
Mixing.
Specifically, the acid solution in S1 and S2 is hydrochloric acid, sulfuric acid or nitric acid, concentration 0.5-4mol/L.
Specifically, the mass ratio of activated matrix material and water is 1:(5~10 in slurries in S2), the volume of acid solution in S2
For the 1-5% of slurry volume.
Specifically, the mass ratio of aniline and activated matrix material is 0.1-1:1 in S2, the mass ratio of aniline and initiator is
1:0.001-0.01.
Specifically, containing Cu in S32+Cu in solution2+Concentration be 50-800mg/L, in S3 overlay film basis material with contain Cu2 +The amount ratio of solution is 30-60g:250mL.
Specifically, the buffer solution in S3 is NaAC-HAC buffer solution.
Specifically, biological material in S4 be rice straw, corn stover, wheat stalk, rice husk, wheat shell, sawdust,
Any one of paper scrap and corncob or any a variety of mixing.
Specifically, the adhesive in S4 is clay or is made of magnesia, calgon, water, silica solution compound viscous
Mixture.
The present invention also provides a kind of adsorption sustained-release fillers for artificial swamp, are prepared by the above method.
Compared with prior art, the beneficial effects of the present invention are:
1) large amount of adsorption, the adsorption capacity of adsorption sustained-release filler provided by the invention are strong, when the pollutants such as nitrogen phosphorus in water inlet
Because content is more can not be complete by the plant absorption on artificial swamp surface layer when, which can be to the pollutant having more
It is effectively adsorbed, so that the water outlet after artificial wetland treatment meets requirement up to standard；
2) adsorption sustained-release filler provided by the invention has slow-release capability, when the pollutants such as nitrogen phosphorus contain less or in water inlet for water inlet
When being unable to satisfy the plant growth on artificial swamp surface layer when measuring low, the adsorption sustained-release filler can will in it before adsorb nitrogen phosphorus
Equal substances are slowly discharged into the very low water body of nitrogen and phosphorus content at root system of plant, to meet the growth demand of plant, in summary
After adsorption sustained-release filler provided by the invention, artificial swamp bears external environment variation (in inflow size variation, water inlet
How much dirt content changes) ability it is stronger；
3) primary raw material for preparing the adsorption sustained-release material is montmorillonite, kaolin and attapulgite and biological material etc.
Cheap products, therefore its lower production costs.
Specific embodiment
Principles and features of the present invention are described below in conjunction with specific embodiment, example is served only for explaining this hair
It is bright, it is not intended to limit the scope of the present invention.
Embodiment 1
S1. it activates: the montmorillonite basis material that partial size is 200-2000 mesh is put into reactor and with 0.5mol/L's
Hydrochloric acid solution is submerged, stir-activating 12h, is centrifugated and is washed to neutrality, dry to get activated matrix material, spare；
S2. overlay film: the activated matrix material 50g in S1 is mixed with 250mL water, is beaten to obtain slurries, and 0.5mol/L is added
Hydrochloric acid solution 12.5mL, sequentially add 5g aniline and 0.05g initiator, stirring at normal temperature reacts 2h, filter, washing, it is dry,
It is ground up, sieved to get overlay film basis material, partial size is 200-2000 mesh；
S3. compound: by the overlay film basis material 30g in S2 and to contain Cu2+The solution 250mL of 50mg/L is mixed, and uses NaAC-
The pH to 6 of HAC buffer solution regulation system, isothermal reaction 4h at 40 DEG C, filtering, filter cake are washed with deionized to Cu2+Content
Dry lower than 0.05mg/L, grinding obtains powdered containing carbon/carbon-copper composite material, and partial size (is equal to or less than 200 mesh below 200 mesh
The partial size of particle)；
S4. be calcined: in parts by weight, by containing in 60 parts of S3, carbon/carbon-copper composite material, (partial size is less than 10 parts of corn stovers
200 mesh), 5 parts of clays and 10 parts of water be uniformly mixed, 4h is then calcined at 150 DEG C, is cooled to room temperature under oxygen-free environment,
Up to the adsorption sustained-release filler for being used for artificial swamp.
Embodiment 2
S1. it activates: the kaolin basis material that partial size is 200-2000 mesh is put into reactor and with the salt of 4mol/L
Acid solution is submerged, stir-activating 1h, is centrifugated and is washed to neutrality, dry to get activated matrix material, spare；
S2. overlay film: the activated matrix material 50g in S1 is mixed with 500mL water, slurries is beaten to obtain, is added 4mol/L's
Hydrochloric acid solution 25mL sequentially adds 50g aniline and 0.05g initiator, and stirring at normal temperature reacts 2-8h, filter, wash, is dry,
It is ground up, sieved to get overlay film basis material, partial size is 200-2000 mesh；
S3. compound: by the overlay film basis material 45g in S2 and to contain Cu2+The solution 250mL of 800mg/L is mixed, and uses NaAC-
The pH to 6 of HAC buffer solution regulation system, isothermal reaction 2h at 60 DEG C, filtering, filter cake are washed with deionized to Cu2+Content
Dry lower than 0.05mg/L, grinding obtains powdered containing carbon/carbon-copper composite material, and partial size is below 200 mesh；
S4. be calcined: in parts by weight, by containing in 70 parts of S3, carbon/carbon-copper composite material, (partial size is less than 15 parts of wheat shells
200 mesh), 7 parts of clays and 15 parts of water be uniformly mixed, 3h is then calcined at 260 DEG C, is cooled to room temperature under oxygen-free environment,
Up to the adsorption sustained-release filler for being used for artificial swamp.
Embodiment 3
S1. it activates: the attapulgite basis material that partial size is 200-2000 mesh is put into reactor and with 2mol/L's
Hydrochloric acid solution is submerged, stir-activating 6h, is centrifugated and is washed to neutrality, dry to get activated matrix material, spare；
S2. overlay film: the activated matrix material 50g in S1 is mixed with 400mL water, slurries is beaten to obtain, is added 2mol/L's
Hydrochloric acid solution 18mL sequentially adds 25g aniline and 0.025g initiator, and stirring at normal temperature reacts 2-8h, filter, wash, is dry,
It is ground up, sieved to get overlay film basis material, partial size is 200-2000 mesh；
S3. compound: by the overlay film basis material 60g in S2 and to contain Cu2+The solution 250mL of 300mg/L is mixed, and uses NaAC-
The pH to 6 of HAC buffer solution regulation system, isothermal reaction 0.5h at 80 DEG C, filtering, filter cake are washed with deionized to Cu2+Contain
Amount is lower than 0.05mg/L, dry, grinding, obtains powdered containing carbon/carbon-copper composite material, and partial size is below 200 mesh；
S4. be calcined: in parts by weight, by containing in 80 parts of S3, carbon/carbon-copper composite material, (partial size is less than 20 parts of rice straws
200 mesh), 10 parts of clays and 20 parts of water be uniformly mixed, 4h is then calcined at 150 DEG C, is cooled to room temperature under oxygen-free environment,
Up to the adsorption sustained-release filler for being used for artificial swamp.
Absorption property detection:
The adsorption sustained-release material prepared by above method is used in urban wastewater treatment, modified montmorillonite,
Kaolin and attapulgite are corresponding in turn to the adsorption sustained-release filler that embodiment 1 to 3 is prepared, and with before modified montmorillonite,
Kaolin, attapulgite absorption property compare, to same sewage after the adsorption treatment of same time period, to nitrogen
The adsorbance of (referring mainly to ammonia nitrogen), phosphorus is tested, and test result is as follows shown in table:
From the data in upper table it is found that the adsorption sustained-release filler prepared by the present invention for artificial swamp is to the nitrogen in sewage
There is stronger adsorption capacity with phosphorus.
Sustained release performance detection:
The adsorption sustained-release material prepared by above method is used in urban wastewater treatment, modified montmorillonite,
Kaolin and attapulgite are corresponding in turn to the adsorption sustained-release filler that embodiment 1 to 3 is prepared.It is operated normally in wet land system
Afterwards, when the autumn and winter plant harvesting phase, the removal of nitrogen phosphorus takes Partial Wetland to fill out mainly by the suction-operated of wet land filler in water inlet
Material, parses ammonia nitrogen, the phosphorus in filler, is measured, and the water outlet in the period is taken to be measured simultaneously.
After above-mentioned autumn and winter plant harvesting, wet season summer is waited until, because water is big, therefore nitrogen phosphorus concentration in water inlet
Lower (the NH of content3- N < 8mg/L, P < 1.0mg/L), the nitrogen phosphorus in water is not enough to allow the more preferable of plant growth, and filler starts at this time
Slow release absorb nitrogen phosphorus for plant growth, at the end of the wet season is fast, take Partial Wetland filler, in adsorption stuffing nitrogen,
Phosphorus is parsed, is measured, and the water outlet in the period is taken to be measured simultaneously, and the result after measurement see the table below:
Data in analysis in table it is found that the wet season because water is big, therefore nitrogen, phosphorus equal size are relatively fewer in intaking, but should
Plant growth is fast when season, therefore nitrogen phosphorus can be fully absorbed and be still had some deficits in intaking, therefore nitrogen phosphorus contains in the water on filler top
Measure it is considerably less, at this time filler can by before it in the nitrogen phosphorus of other periods such as harvest time absorption to upper part region slow release,
For plant absorption.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the adsorption sustained-release filler for artificial swamp, which comprises the steps of:
S1. it activates: will be submerged in the basis material investment reactor after screening and with acid solution, stir-activating 1-12h, from
The heart separates and is washed to neutrality, dry to get activated matrix material, spare；
S2. overlay film: the activated matrix material in S1 is mixed with water, is beaten to obtain slurries, and acid solution is added, sequentially adds aniline
And initiator, stirring at normal temperature react 2-8h, filter, washing, drying, are ground up, sieved to get overlay film basis material；
S3. compound: by the overlay film basis material in S2 and to contain Cu2+Solution mixing, with the pH to 6,40- of buffer solution regulation system
The Cu into washing filtrate is washed with deionized in isothermal reaction 0.5-4h at 80 DEG C, filtering, filter cake2+Content is lower than 0.05mg/L,
Dry, grinding obtains powdered containing carbon/carbon-copper composite material；
S4. it is calcined: in parts by weight, carbon/carbon-copper composite material, 10-20 parts of biological materials, 5-10 will be contained in 60-80 parts of S3
Part adhesive and 10-20 parts of water are uniformly mixed, and 2-4h is then calcined at 150-400 DEG C, is cooled to room under oxygen-free environment
Temperature is to get the adsorption sustained-release filler for artificial swamp；
Basis material in step S1 is any one or any a variety of mixing in montmorillonite, kaolin and attapulgite.
2. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
Acid solution in S1 and S2 is hydrochloric acid, sulfuric acid or nitric acid, concentration 0.5-4mol/L.
3. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
The mass ratio of activated matrix material and water is 1:(5~10 in slurries in S2), the volume of acid solution is the 1- of slurry volume in S2
5%.
4. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
The mass ratio of aniline and activated matrix material is 0.1-1:1 in S2, and the mass ratio of aniline and initiator is 1:0.001-0.01, institute
Stating initiator is one of sodium peroxydisulfate, potassium peroxydisulfate and ammonium persulfate or a variety of.
5. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
Contain Cu in S32+Cu in solution2+Concentration be 50-800mg/L, in S3 overlay film basis material with contain Cu2+The amount ratio of solution is
30-60g:250mL。
6. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
Buffer solution in S3 is NaAC-HAC buffer solution.
7. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to claim 1, which is characterized in that
Biological material in S4 is in straw straw, corn stalk, wheat straw, rice husk, wheat shell, sawdust, paper scrap and corncob
Any or any a variety of mixing.
8. a kind of preparation method of adsorption sustained-release filler for artificial swamp according to any one of claims 1 to 7,
It is characterized in that, the adhesive in S4 is clay or the composite adhesive being made of magnesia, calgon, water, silica solution.
9. a kind of adsorption sustained-release filler for artificial swamp, which is characterized in that described in any item by claim 1 to 8
Method is prepared.
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| CN110357198A (en) * | 2019-06-11 | 2019-10-22 | 武汉兴天宇环境股份有限公司 | A kind of adsorbent material and preparation method thereof for Low Concentration Ammonia Containing Wastewater processing |
| CN115465943A (en) * | 2022-09-21 | 2022-12-13 | 王卓 | Constructed wetland nitrogen and phosphorus removal filler with slow-release carbon material and preparation method thereof |
| CN116119833B (en) * | 2022-11-29 | 2023-09-08 | 嘉兴沃特泰科环保科技股份有限公司 | Nutrient for water recovery system and preparation method and application thereof |
| CN116409880A (en) * | 2023-03-06 | 2023-07-11 | 商洛学院 | Preparation method for preparing high-performance constructed wetland filler by using tailings |
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Denomination of invention: An adsorption slow-release filler for constructed wetland and its preparation method Effective date of registration: 20230303 Granted publication date: 20190618 Pledgee: Bank of China Limited Wuhan Hanyang sub branch Pledgor: WUHAN FUND ENVIRONMENT PROTECTION Co.,Ltd. Registration number: Y2023420000088 |