CN104587976B - Dephosphorization adsorption capsule grains for water treatment and preparation method thereof - Google Patents
Dephosphorization adsorption capsule grains for water treatment and preparation method thereof Download PDFInfo
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- CN104587976B CN104587976B CN201510037138.3A CN201510037138A CN104587976B CN 104587976 B CN104587976 B CN 104587976B CN 201510037138 A CN201510037138 A CN 201510037138A CN 104587976 B CN104587976 B CN 104587976B
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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
- B01J20/02—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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention provides dephosphorization adsorption capsule grains for water treatment and a preparation method thereof. The preparation method comprises the following steps of reacting chitosan and molysite by taking water as a reaction medium so as to obtain colloid; adding the colloid into an alkaline solution, and standing to obtain a system containing dephosphorization adsorption capsule grains. According to the invention, molysite and chitosan react, and the colloid obtained by reaction is added into the alkaline solution so as to obtain solid dephosphorization adsorption capsule grains, so that the problem that in the traditional method, molysite is easily dissolved in water, and the hydrolyzed molysite forms a great amount of floc alumen ustum with pollutants to further cause secondary pollution is solved. After phosphorus removal of the product grains prepared by the invention, the product grains can act as a slow release phosphatic fertilizer to be applied to the field of agriculture and horticulture. With the dephosphorization adsorption capsule grains prepared by the invention, phosphorus in sewage and river and lake water is recycled and utilized, waste is turned into wealth, and thus good economic benefit, as well as good environment and ecological benefits are achieved.
Description
Technical field
The invention belongs to water treatment field, and in particular to a kind of dephosphorization absorption capsule particle and its preparation for water process
Method.
Background technology
While the mankind enjoy the benefit that water brings in life and production, the body that also feeds water brings pollution and destroys water ring
Border, phosphorus is exactly one of pollutant therein.Sanitary sewage is a main source of phosphorus pollution, and the phosphorus entered in water body there are about
64% from sanitary sewage, and mankind's dung urinates the discharge capacity of total phosphorus in gross contamination emission up to 5.24kg/ (man-year), the whole world
About 1.38 hundred million tons of annual phosphorus ore yield, has 12% for producing detergent, and detergent row's phosphorus amount accounts for whole sanitary sewage phosphorus
19% or so of discharge capacity.It is substantial amounts of to discharge phosphorus in water body, to water source, soil, pollute, health is constituted and is endangered
Evil, while the way for exploiting rock phosphate in powder simply is also unsustainable, and enters the phosphorus in water and cannot utilize well, this
The wasting of resources is not only caused also to bring problem of environmental pollution.Phosphorus pollution how is solved, becomes puzzlement sewage disposal row for many years
The a great problem of industry.Therefore, seek cost-effective method to recycle phosphorus, the development of water treatment field can not only be promoted,
To also important impact be produced to the sustainable development of real economy, society.
For a long time, in various dephosphorization chemical agents, molysite is one of modal medicament, but because molysite is soluble in
Water forms liquid, and substantial amounts of flco alumen ustum is formed with pollutant after its hydrolysis, can be any with current compared with the case of light in flco
Discharge, not only causes serious secondary pollution, while and being the serious waste to resource to environment.
The content of the invention
It is an object of the invention to provide capsule particle and preparation method thereof is adsorbed in a kind of dephosphorization for water process.
Dephosphorization absorption capsule particle provided by the present invention is prepared by the method comprising the following steps：
With water as reaction medium, shitosan is reacted with molysite, obtain viscolloid；The viscolloid is added
To in alkaline solution, obtain adsorbing the system of capsule particle containing dephosphorization after standing.
In the reaction, the molysite adds reaction system in the way of molysite aqueous solution.
In the molysite aqueous solution, the mass concentration of iron ion is 0.2%-0.4%, concretely 0.4%.
The molysite is selected from following at least one：Iron chloride, ferric nitrate, ferric sulfate, poly-ferric chloride and bodied ferric sulfate.
The shitosan is the shitosan that deacetylation is 85%-95%.
In the reaction, the shitosan adds reaction system in the way of the Chitosan powder.
The shitosan is 1-2 with the mass ratio of the molysite:0.95-1.7, concretely 2:0.95.
The temperature of the reaction is 40 DEG C -70 DEG C, and concretely 60 DEG C, the time of the reaction is -3 hours 1 hour, tool
Body can be 3 hours.
In order to ensure the homogeneity of reaction system, the reaction is carried out under agitation.
The alkaline solution is inorganic base aqueous solution.
The inorganic base is selected from following at least one：NaOH, potassium hydroxide, sodium carbonate and potassium carbonate.
In the alkaline solution, the molar concentration of the inorganic base is 0.5-1mol/L, concretely 0.7mol/L.
The viscolloid is 0.5L-1L with the proportioning of the alkaline solution:2L-3L, concretely 1L:2L.
The viscolloid is added in the alkaline solution by the way of being added dropwise.
The dropwise addition is：It is introduced in tubule with mechanical pump after the viscolloid is cooled down, under agitation by the stickiness
Colloid is dropwise instilled in the alkaline solution.
The internal diameter of the tubule is usually 0.5-2 millimeters, concretely 1.2 millimeters, and the speed of the dropwise addition is that 2-3 drops are every
Second, the ozzle of the tubule is 16 centimetres -30 centimetres, concretely 20 centimetres with the distance of the alkaline solution liquid level.
The time of the standing is -30 minutes 10 minutes, concretely 30 minutes.
Said method also includes the system for adsorbing capsule particle containing dephosphorization being carried out into separation of solid and liquid and dividing solid-liquid
The step of obtaining wet shape dephosphorization absorption capsule particle is cleaned with water from the solid for obtaining.
The liquid obtained after the separation of solid and liquid can be reused for configuring alkaline solution.
The cleaning can be carried out 3-6 time, and cleaning is stopped when the pH value of the cleaning fluid for measuring is 7.0-7.5.
The cleaning fluid can be reused for configuring alkaline solution after collecting.
Said method can also be further included to be dried the wet shape dephosphorization absorption capsule particle and obtain dry shape dephosphorization
The step of absorption capsule particle.
The temperature of the drying is 50 DEG C -70 DEG C, concretely 70 DEG C.
The time of the drying is 180min-300min, concretely 240min.
The wet shape prepared by said method/dry shape dephosphorization absorption capsule particle falls within protection scope of the present invention.
The average grain diameter of the wet shape dephosphorization absorption capsule particle is 3mm-5mm.
The average grain diameter of the dry shape dephosphorization absorption capsule particle is 1mm-1.8mm.
The wet shape/application of the dry shape dephosphorization absorption capsule particle in water process falls within protection scope of the present invention.
The water concretely sewage, river course and Lake Water.
The present invention is reacted molysite with shitosan, then the viscolloid that reaction is obtained is added in alkaline solution,
Obtain dephosphorization absorption capsule particle solid, it is to avoid molysite is soluble in water in conventional method, can be formed greatly with pollutant after hydrolysis
The flco alumen ustum of amount, causes the problem of secondary pollution.
This products application can be removed in water treatment field to the phosphorus in water body, phosphorus pollution in removing water body is reached
Effect.Moreover, because shitosan has biocompatibility, biological degradability and the characteristic such as nontoxic, extensively should
For biomedicine field and agriculture field, therefore, product particle, can conduct after the removal for completing phosphorus by obtained in the present invention
A kind of slow-release phosphate fertilizer is applied to agricultural and horticultural field.Phosphorus in such sewage or water body can be used, and turn waste into wealth, not only
There is good economic benefit, and with good environment and ecological benefits.The present invention gives one kind shitosan and molysite
The method that capsule particle is adsorbed in production dephosphorization, process is workable, and the utilization rate of raw material is high.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is wet shape dephosphorization absorption capsule particle (left figure) that the embodiment of the present invention 1 is prepared and dry shape dephosphorization absorption
The photo of capsule particle (right figure).
Fig. 3 be the embodiment of the present invention 1 prepare dry shape dephosphorization absorption capsule particle multiplication factor be 30,140,
Scanning electron microscopic picture under 370 and 600 times obtained by scanning.(using electron scanning Electronic Speculum instrument to dry shape capsule particle surface shape
Before state observation, upper sem observation after metal spraying process is carried out to capsule particle, is taken pictures, the multiplication factor of B1 is 30 times, the times magnification of B2
Number is 140 times, the multiplication factor of B3 is 370 times, the multiplication factor of B4 is 600 times)
Fig. 4 is the section SEM pictures (270 times) that capsule particle is adsorbed in the dry shape dephosphorization that the embodiment of the present invention 1 is prepared.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental technique used in following embodiments if no special instructions, is conventional method；Institute in following embodiments
Reagent, material etc., if no special instructions, commercially obtain.
Shitosan employed in following embodiments for Chemical Reagent Co., Ltd., Sinopharm Group product, deacetylation >=
90%.
Embodiment 1, dephosphorization adsorbs the preparation of capsule particle
1) viscolloid is prepared：
It is by the mass concentration that 9.5 kilograms of ferric chloride hexahydrate is dissolved in the prepared iron ion of water in acid-proof porcelain reactor
0.4% ferric chloride hexahydrate solution, under stirring, slowly adds in the acid-proof porcelain reactor for filling ferric chloride hexahydrate solution
Plus 20 kilograms of Chitosan powder, spray water drops to cumulative volume for one cubic metre, makes pasty state and continues to stir 3 little at 60 DEG C
When, fully reaction obtains bronzing viscolloid；
2) cooling drop glue：
Viscolloid mechanical pump after cooling is introduced in the tubule that internal diameter is 1.2 millimeters, with the speed that 2～3 drops are per second
Degree dropwise instills concentration for (tubule ozzle is 20 centimetres with the distance of alkali lye liquid level), institute in the sodium hydroxide solution of 0.7mol/L
It is 1L that viscolloid is stated with the volume ratio of sodium hydroxide solution:2L, and be stirred, 30 minutes are stood after being added dropwise to complete, then
Separation of solid and liquid is carried out, solid is collected standby；
3) product treatment
By obtained solid cleaned with running water to pH value be 7.0-7.5 when stop cleaning, cleaning fluid collect after, can be again
For making alkaline solution, separation of solid and liquid obtains wet shape absorption capsule particle (average grain diameter is 3-5 millimeters) storage.As needed
Drying type capsule particle is wanted, the product after cleaning is dried into 240min at a temperature of 70 DEG C, obtain drying type suction
Attached capsule particle (average grain diameter is 0.9～1.5mm).In terms of butt, in the absorption capsule particle, the content of iron is 240mg/
g。
The dry and wet state for adsorbing capsule particle is taken pictures using Electrofax, and capsule is measured with high accuracy steel ruler
Grain diameter.
Fig. 2 is wet shape dephosphorization absorption capsule particle (left figure) and dry shape dephosphorization absorption capsule particle (right figure) for preparing
Photo.
As shown in Figure 2：Wet shape capsule particle and dry shape capsule particle have larger difference in color.Wet shape capsule particle is several
It is spherical, color takes on a red color, uniform color, surface is smooth；Meanwhile, the closing space, surface pore inside particle with
And smooth surface has quite a few water, that is, water, interstitial water and particle surface attached water are closed, the water of these multi-forms
Presence increases the volume of particle so that capsule particle integrally presents saturation state, and wet shape capsule particle particle diameter is about 3～
5mm, the left figure seen in Fig. 2.
Dry shape capsule particle is irregular spherical, and many concave-convex surfaces, ellipticity mostly, in the environment of vacuum drying,
As the evaporation of moisture, chelate are gradually concentrated, particle volume reduction, local chrominance is caused to be deepened in bronzing, shape is enriched；
Simultaneously as static drying is used, particle and the mutual stress of bottom refined net in dry run, so, drying type glue
Capsule particle surface many places are in plane, and dry shape capsule particle particle diameter is about 0.9～1.5mm, the right figure seen in Fig. 2.
Capsule particle surface is adsorbed to dephosphorization under the accelerating potential of 20.0kv using JSM-7001F electron scanning Electronic Speculum instrument
Form carries out electron microscopic observation.
Fig. 3 is the dry shape dephosphorization absorption capsule particle for preparing in the case where multiplication factor is for 30,140,370 and 600 times
Scanning electron microscopic picture obtained by scanning is (before adopting electron scanning Electronic Speculum instrument to dry shape capsule particle surface morphologic observation, to capsule
Particle carries out after metal spraying process sem observation, takes pictures, and the multiplication factor of B1 is 30 times, and the multiplication factor of B2 is 140 times, B3 is put
Big multiple is 370 times, the multiplication factor of B4 is 600 times).
As shown in Figure 3：Using the configuration of surface of electron microscopy study capsule particle, the basic rule of capsule particle form can be obtained
Rule：Dry shape capsule particle is the space prosperity, surface irregularity by chelate concentration together, with distributed architecture in the same direction
Capsule particle.
Pure chitosan under nature is substantially the polyamino glucose polymer of non-hole, through the place of the present invention
After reason, it can be observed that obtained capsule particle presents a large amount of ducts and pore structure is obvious.
The capsule particle is cut into into two parts, it is same from section it is observed that capsule particle inside has simple hole
Gap texture, is shown in Fig. 4.
In sum, the shitosan in obtained absorption capsule particle there occurs quite compared with pure chitosan in form
Big change.The adsorbent of obtained loose structure is more beneficial for improving adsorption effect.
The evaluation of the dephosphorization absorption property of embodiment 2, dephosphorization absorption capsule particle
The assay method of adsorption capacity is:The adsorbent for taking mass M is put in conical flask, is then added in the conical flask
Concentration C0For 100mgPO4 3-/ L, measures the potassium dihydrogen phosphate dissolving of volume V, in isothermal vibration device by adsorbent dosage 2g/L
In adsorbed, adsorption time is 24h, and adsorption temp is 25 DEG C, after absorption terminates, PO in solution after measurement absorption4 3-Concentration
Ce.Phosphorus concentration is determined according to GBT11893-1989, adsorbs apparent adsorption capacity q (mg/g)=V* (C of capsule particle0-Ce)/M
Table 1, the dry shape dephosphorization of embodiment 1 adsorb the data of capsule particle
| Index | Data |
| BET specific surface area | 4.3(㎡/g) |
| Pore volume | 0.006(ml/g) |
| Aperture | 5.019(nm) |
| Adsorption capacity (2g/L dosages, 31.95mg P/L) | 8.93(mg P/g) |
| Shitosan percentage by weight | 76wt% |
| Grain density | 1.6g/cm3 |
| Grain diameter | 0.9-1.5mm |
Comparative example 1
" Ma Weichao, Ma Jun, Han Bangjun, nascent state hydrated ferric oxide removes the effect research of phosphate radical in eliminating water to document, China
Water supply and drainage, 2 months 2010 phase of volume 26 the 3rd " discloses a kind of common hydrated ferric oxide HIO, and its preparation is comprised the following steps：
A, deionized water prepare the ferric chloride solution of 0.1mol/L；B, with the sodium hydroxide solution of 160g/L it is titrated to pH at normal temperatures
It is worth for 11 or so, is allowed to heavy fixed reaction, mixed liquor is centrifuged into (5000r/min), abandoning supernatant, deionized water is clear
Wash, be centrifuged again, be repeated several times until the pH of washings is close to neutrality, heavy earnest is dried to constant mass at 105 DEG C, obtain
To metaborate monohydrate iron oxide adsorbent.Its adsorbance is only 6mg/g.Compared with the adsorbance (8.93mg/g) in the present embodiment
Compared with, although bibliography is simple hydrated ferric oxide, but its adsorbance is still than the adsorption particle for preparing of the invention
Adsorbance is little a lot, and both architectural differences are big.
Comparative example 2
CN201210091217.9 discloses a kind of preparation method of dephosphorization activated carbon containing iron adsorbent, including following step
Suddenly:A, with salt acid soak 14～14h of Powdered Activated Carbon, cleaned with 90～100 DEG C of distilled water again after filtration, at 100～105 DEG C
It is dried；B, with acid with strong oxidizing property solution impregnation step A of mass content 20%～45% gained dry activated carbon 12～
24h, then filtered, cleans constant to pH, then at 100～105 DEG C of dryings 6～12 hours；C, by step B gained activated carbon with
The inorganic molysite solution of 0.1～0.5mol/L is mixed, and in 110～120 DEG C 24～48h is dried, then is washed away not with distilled water
The iron oxide of load, continues to be dried at 100～105 DEG C, obtains dephosphorization activated carbon containing iron.The dephosphorization activated carbon containing iron absorption
The saturated adsorption capacity of agent is 7～10mg/g (1～1.5g/L dosages, 20～30mg PO4 3-/L).Although
The saturated extent of adsorption of CN201210091217.9 is close to the present embodiment, and compared with the method in the present embodiment, its needs is lived
Property charcoal as medium, preparation process is relatively cumbersome, expend the time it is more, consume energy it is larger, used the strong oxidizing property of higher concentration
Acid solution easily produces contaminant by-products, while also using higher inorganic molysite concentration, economy is poor, and phosphorus and iron
Reaction to be produced and easily shed into solution after precipitation, causes phosphorus to reclaim more difficult.And present invention preparation is capsule, produce after phosphorus absorption
Raw precipitation is wrapped up by capsule, easily realizes that phosphorus is reclaimed using rear.
Claims (8)
1. the preparation method of capsule particle is adsorbed in a kind of dephosphorization, is comprised the steps：With water as reaction medium, shitosan and iron are made
Salt is reacted, and obtains colloid；The colloid is added in alkaline solution, obtains adsorbing capsule particle containing dephosphorization after standing
System；
The shitosan is 1-2 with the mass ratio of the molysite:0.95-1.7；
The temperature of the reaction is 40 DEG C -70 DEG C, and the time of the reaction is -3 hours 1 hour；
The alkaline solution is inorganic base aqueous solution；
The inorganic base is selected from following at least one：NaOH, potassium hydroxide, sodium carbonate and potassium carbonate；
The molysite is selected from following at least one：Iron chloride, ferric nitrate, ferric sulfate, poly-ferric chloride and bodied ferric sulfate.
2. method according to claim 1, it is characterised in that：In the alkaline solution, the molar concentration of the inorganic base
For 0.5mol/L-1mol/L.
3. method according to claim 1 and 2, it is characterised in that：The colloid is with the proportioning of the alkaline solution
0.5L-1L:2L-3L。
4. method according to claim 1 and 2, it is characterised in that：The colloid is added to described by the way of being added dropwise
In alkaline solution；
The dropwise addition is：Colloid after cooling is introduced in tubule with mechanical pump, under agitation the colloid institute is dropwise instilled into
In stating alkaline solution；
The internal diameter of the tubule is 0.5-2 millimeters；
The speed of the dropwise addition is that 2-3 drops are per second；
The ozzle of the tubule is 16 centimetres -30 centimetres with the distance of the alkaline solution page.
5. method according to claim 1 and 2, it is characterised in that：The time of the standing is -30 minutes 10 minutes.
6. method according to claim 1 and 2, it is characterised in that：Methods described is also included described containing dephosphorization absorption
The solid that the system of capsule particle carries out separation of solid and liquid and obtains separation of solid and liquid is cleaned with water and obtains wet shape dephosphorization absorption capsule
The step of particle；
Methods described is still further comprised to be dried the wet shape dephosphorization absorption capsule particle and obtains dry shape dephosphorization absorption glue
The step of capsule particle.
7. the dephosphorization absorption capsule particle that the method by any one of claim 1-6 is prepared, it is characterised in that：It is described
Dephosphorization absorption capsule particle is that capsule particle is adsorbed in wet shape dephosphorization, and its average grain diameter is 3mm-5mm；
The dephosphorization absorption capsule particle is that capsule particle is adsorbed in dry shape dephosphorization, and its average grain diameter is 1mm-1.8mm.
8. dephosphorization absorption application of the capsule particle in water process described in claim 7, wherein, the water be sewage, river course and
Lake Water.
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