CN104609374A - Preparation method and application of layered double metal hydroxide bloom alga remover - Google Patents
Preparation method and application of layered double metal hydroxide bloom alga remover Download PDFInfo
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- CN104609374A CN104609374A CN201510037864.5A CN201510037864A CN104609374A CN 104609374 A CN104609374 A CN 104609374A CN 201510037864 A CN201510037864 A CN 201510037864A CN 104609374 A CN104609374 A CN 104609374A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/006—Compounds containing, besides zinc, two ore more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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Abstract
The invention discloses a preparation method and an application of a layered double metal hydroxide bloom alga remover. According to the bloom alga remover, a bivalent and trivalent metal combination reacts with alkali to prepare layered double metal hydroxide, and negatively charged algal cells in water are electrostatically adsorbed and flocculated by utilizing a characteristic that laminates of the layered double metal hydroxide are positively charged, so that algae in the water are removed; the prepared layered double metal hydroxide is high in charge density of the laminates, 0.758 nm in interlayer spacing and 20-50 microns in powder size, and the bloom alga remover is good in alga removal performance; the removal rate of the layered double metal hydroxide to algal chlorophyll a is more than 94.62%; the preparation method adopted by the invention is simple, the obtained powder material is good in crystal form and morphology, the alga removal process is simple, formed algal flocs are good in settling performance and can be separated from the water quickly, and the alga remover is low in consumption and low in cost.
Description
Technical field
The invention belongs to field of functional materials, relate to a kind of preparation method and application thereof of layered double hydroxide wawter bloom algae remover.
Background technology
Layered double hydroxide is a kind of type material with multiple properties such as anionresin, adsorptivity, thermostability, memory effect, soda acid bi-functional and catalytics.Domestic and international research shows, it have been got everything ready potential using value at numerous areas such as catalysis, ion-exchange and absorption, medicine, biologies.In recent years, it also receives much concern in water treatment field, and research finds that it has fine removal effect to anionic pollutant and heavy metal ion.
Along with the quickening of socioeconomic development and process of industrialization, there is increasing nitrogen and phosphorus pollution material to enter water body, result in the aggravation of water body eutrophication degree and the continuous expansion of scope.In water body, the Fast-propagation growth of blue-green algae, reduces transparency and the dissolved oxygen of water body, hydrocoles death by suffocation, produces niff, affect sense organ, the more important thing is Algae toxins that algae discharges also serious threat the health of the mankind and hydrocoles.Drinking water source algae breaks out and the difficulty of water treatment and economic operation cost is increased all to some extent.Therefore, people urgently find a kind of safety, and economical, the algae-removing method of efficient pollution-free cracks this global difficult problem.
At present, a lot of to the minimizing technology of wawter bloom algae, sum up and get up to mainly contain following a few class:
1 Physical is except algae
Physical removes algae means except algae generally includes the physics such as air supporting, filtration, micro-filtration, ultrasonic wave, absorption method.
A, By Bubble-floating Method: algae density is less, flocs unit not easily precipitates this unfavorable factor to adopt By Bubble-floating Method to overcome.The speed utilizing air supporting to make flocs unit shift to water surface removal is removed fast a lot than precipitation.But the algae-residue that this method is formed is difficult to process, and stink weight near air flotation pool, operating environment is poor.Air supporting is gone to toward needing prechlorination in addition, jeopardizes the security of drinking-water.The removal effect of air supporting simultaneously to turbidity is poor, can affect subsequent technique treatment effect.
B, filtration method: direct filtration treatment system, the feature simple with its technical process, reduced investment, working cost are low and extremely producing and the attention of design department.At 20th century six the seventies, this method has been commonly used to the process of algae-containing water, and its technology is feasible by facts have proved, but requires high to operation and management level, slightly slips up, just may affect effluent quality.Direct filtration is not suitable for processing containing the high water of algae amount, should increase settling tank and settling pond, but also may occur the situation of the algae content overproof of filter tank water outlet like this, need process further before filtering basin.And algae easily causes filter bed to block, cause that workload is large, cycle time is long, and working cost is high, because which limit the application of the method.
C, supersonic method: utilize hyperacoustic mechanical vibration, acoustic streaming and cavitation effect to cause the damage of tissue of biological cells, fracture or fragmentation, to reach the object suppressing algal grown.But this method can impact the other biological in water body, and greatly accelerates the release of Algae toxins, and running cost is high.
D, absorption method: utilize gac, the adsorbent such as clay remove algae.Generally speaking absorption method can remove wawter bloom algae preferably.Gac is a ripe effective means for the organic pollutant removed in water.Gac is a kind of porous material, to organic removal mainly by micro-porous adsorption effect, can be obtained the removal effect of good algae and Algae toxins, but there is the higher shortcoming of running cost by absorption.Clay adsorption removes algae has significant effect to improving Algae toxins in water quality condition, removal water.But clay itself except algae effect unsatisfactory, generally will by modification, properties-correcting agent easily causes secondary pollution to water body.
2 chemical methods are except algae
A, alga removalby coagulation
The coagulating agent that alga removalby coagulation is conventional has aluminium salt (polymeric aluminum sulfate silicate, polymerize aluminum chloride, Tai-Ace S 150 etc.) and molysite class (ferric sulfate of polymerized silica, polysilicate ferric chloride etc.).Due to alga cells secretion dissolved organic matter, the outer organism of born of the same parents is primarily of nitrogenous substances and pentose gelatin substance composition, the saccharic acid secreted by algae and uronic acid can and coagulating agent in molysite and aluminium salt formation complex compound and be unfavorable for surely de-, therefore it is low that conventional coagulant sedimentation removes algae efficiency, settling of floccus poor performance, need be strengthened to improve except algae efficiency to it.
B, prechlorination method are except algae
Preoxidation refers to, before coagulation operation, add oxygenant, in order to remove organic micro-pollutants, the stink in former water, or plays the water purification operation of Coagulation aiding.Prechlorination method has good treatment effect to algae and water, but prechlorination makes disinfection byproduct (DBP) in water increase, unfavorable to HUMAN HEALTH, has some algae to produce stink after prechlorination.In addition, the pH of high algae phase water is high, ClO
-many, always make the clearance of some algae not increase with the increase of chlorine dosage.
C, chemical agent kill algae
Utilizing chemical agent to kill algae is use at most both at home and abroad at present, is also the algae removal technology of relative maturity.Have except algae speed is fast, the advantage of successful is a kind of economical and effective, simple and easy to do algae-removing method.But because chemical agent also has killing action to other biology, the release of Algae toxins can be accelerated simultaneously, affect the safety of aquatic ecosystem, easily cause the features such as secondary pollution, limit its development and application.Such as, algicide copper sulfate most widely used at present, it is used for source water and kills algae, but copper sulfate can cause Algae toxins accelerated release in vitro, and in water body, the rising of mantoquita concentration also endangers HUMAN HEALTH.
3 biological processes are except algae
The vital movement of biology of the biology that biological process is cultivated except algae utilizes or cultivation, inoculation, transforms water pollutant, degrades and transferance, thus make a kind of method that water body environment health is restored.Also there are some algae-lysing microorganism, as bacterium, fungi, virus etc. simultaneously.Most algae-lysing bacterium can secrete the outer material of born of the same parents, plays suppression or killing action to host algae.The advantages such as safety, expense are low, non-secondary pollution that utilize biological process control algae to have, but also to have the algae removal action period long simultaneously, the shortcomings such as algaecidal rate is relatively low.
4 lower temperature plasma technologies
Lower temperature plasma technology is a high-level oxidation technology of new rise in the last few years.But its result of study is the random experiments result of the fragmentary dispersion that each investigator obtains under special experiment condition, have no systems analysis test, reaction result is difficult to the bottleneck controlling to become industrial applications.
Summary of the invention
Above-mentioned various algae-removing methods have its respective merits and demerits.For the deficiency of existing algal tufa treatment agent and method, the object of this invention is to provide a kind of preparation method and application thereof of layered double hydroxide wawter bloom algae remover.
Its preparation method is simple, and the powder crystalline phase of preparation is grown complete, and purity is high, pattern rule, size uniform.The algae-removing method of layered double hydroxide is simple, and except algae efficiency is high, without chemical pollution, cost is low.
The preparation method of a kind of layered double hydroxide wawter bloom algae remover provided by the invention, comprises the following steps:
(1) by mol ratio M
2+/ M
3+be that the soluble divalent metal salt of 2 ~ 3.5 ︰ 1 and trivalent metal salt are dissolved in distilled water and are mixed with mixing salt solution, by mol ratio OH
-/ CO
3 2-be NaOH and the anhydrous Na of 2 ~ 3 ︰ 1
2cO
3be dissolved in distilled water and be made into mixed ammonium/alkali solutions;
(2) be that the mixed ammonium/alkali solutions of 1.8 ~ 1 ︰ 1 and mixing salt solution dropwise join in the reaction vessel of vigorous stirring simultaneously by volume ratio, keep slurry temperature in reaction vessel constant in 65 ~ 85 DEG C in dropping process, in dropping process maintenance reactor, slurry pH value is in 9.8 ~ 10.3 scopes, after dropwising, continue constant temperature and stir 1h, make abundant hybrid reaction;
(3) reacted slurries are bathed ageing 6 ~ 16h at 50 ~ 70 DEG C of Water Unders;
(4) resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain layered double hydroxide powder.
In step (1), soluble divalent metal salt is ZnSO
47H
2o, Mg (NO
3)
26H
2o or Cu (NO
3)
23H
2o; Soluble trivalent metal salt is Al (NO
3)
39H
2o.
The layered double hydroxide powder that step (4) obtains, interlamellar spacing is 0.758nm, and powder size is 20 ~ 50 μm.
The present invention also provides a kind of described layered double hydroxide wawter bloom algae remover to be applied to wawter bloom except algae, and from water, algae is removed in flocculation.
Described layered double hydroxide wawter bloom algae remover application: first add 20 ~ 30mg/L layered double hydroxide in water, then rapid stirring mixing 3min under 250r/min condition, low rate mixing 10 min under 30r/min condition again, last quiet heavy 10min, the algae flco natural sedimentation of generation.
Layered double hydroxide of the present invention has following characteristics except algae method, chemical algae removing method and biological removing compared with algae method except method and the physics used at present of algae:
1, layered double hydroxide consumption is few, and cost is low, and the treatment time is short, and algae clearance is high, instant effect.The algae floc settling velocity formed is fast, most at 8 ~ 12mm/s, reaches as high as 20mm/s.
2, without chemical pollution: layered double hydroxide mainly relies on positively charged veneer structure and electronegative frustule effect except algae, can not cause cell rupture and discharge Algae toxins polluted-water.It had both had the high-speed feature of chemical algae removing efficiency, turn avoid the secondary chemical pollution problem that chemical algae removing technology exists.
3, simple to operate, enforcement convenience, uses conventional whipping appts, economical and practical.
Layered double hydroxide is a kind of inorganic functional material of safety environment protective, removes wawter bloom algae, have efficient, safe feature, alternative various algal tufa treatment agent with it, except algae has popularizing application prospect in the water of body eutrophication field.
Accompanying drawing explanation
Fig. 1 is the XRD figure of zinc-aluminium layered double hydroxide powder prepared by the present invention.
Fig. 2 is the FTIR figure of zinc-aluminium layered double hydroxide powder prepared by the present invention.
Fig. 3 is the adsorption-desorption curve of zinc-aluminium layered double hydroxide powder prepared by the present invention.
Fig. 4 is the graph of pore diameter distribution of zinc-aluminium layered double hydroxide powder prepared by the present invention.
Fig. 5 and Fig. 6 is the SEM figure of zinc-aluminium layered double hydroxide powder prepared by the present invention.
Fig. 7 is the SEM figure of the algae flco generated after the zinc-aluminium layered double hydroxide powder handling algae-containing water prepared of the present invention.
Have seven characteristic diffraction peaks from the visible zinc-aluminium layered double hydroxide of Fig. 1 XRD figure, peak shape is symmetrical, sharp-pointed, and illustrate that crystal formation is grown, calculating interlamellar spacing with Bragg equation is 0.758nm.
Type and their positioning scenarios of key is formed from the information of the ionic nature existed between Fig. 2 TIR figure visible layer and negatively charged ion.At 3460cm
-1and 758cm
-1neighbouring absorption corresponds to the absorption peak of the stretching vibration of hydroxyl and the flexural vibration generation of water, and the absorption that spectrum produces in lower wave number district corresponds to the lattice vibration of laminate lattice, 1360cm
-1neighbouring absorption peak is interlayer CO
3 2-charateristic avsorption band, 3100cm
-1the weak absorbing acromion at place corresponds to water molecules and interlayer CO
3 2-form the absorption peak of hydrogen bond.
There is less hysteresis loop in adsorption-desorption curve as seen from Figure 3, illustrates that this material comprises mesoporous.
The pore size distribution situation of this material can be obtained from Fig. 4 graph of pore diameter distribution.
Assembled from Fig. 5 zinc-aluminium layered double hydroxide by tabular crystal, granule-morphology is like layer column.
Scheme visible powder granule rule from Fig. 6 powder SEM, size is 20 ~ 50 μm.
Scheme visible flaky material from Fig. 7 flco SEM and be attached to frustule surface, lamella is combined well with cell.
Embodiment
embodiment 1:
Step 1: the ZnSO by mol ratio being 2.7 ︰ 1
47H
2o and Al (NO
3)
39H
2o mixing is dissolved in distilled water and is mixed with mixing salt solution, is separately NaOH and the anhydrous Na of 2 ︰ 1 by mol ratio
2cO
3mixing is dissolved in distilled water and is made into mixed ammonium/alkali solutions;
Step 2: dropwise join in the reaction vessel of vigorous stirring while of being mixed ammonium/alkali solutions and the mixing salt solution of 1.8 ︰ 1 by volume ratio, slurries constant temperature 75 DEG C in reaction vessel is kept in dropping process, in dropping process maintenance reactor, slurry pH value is 9.8 ~ 10.3, after dropwising, continue constant temperature and stir 1h, make its abundant hybrid reaction;
Step 3: by reacted slurries at 65 DEG C of Water Under bath ageing 6h;
Step 4: resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain zinc-aluminium layered double hydroxide sample (1. number).
This zinc-aluminium layered double hydroxide sample (1. number) is for except algae, material dosage is 25mg/L, then rapid stirring mixing 3min under 250r/min condition, then under 30r/min condition low rate mixing 10 min, last quiet heavy 10min is 4.68 × 10 to plan post spore algae density
8after the water sample of individual/L processes, the clearance of chlorophyll a is more than 94.62%.
embodiment 2:
Step 1: the ZnSO by mol ratio being 2.5 ︰ 1
47H
2o and Al (NO
3)
39H
2o mixing is dissolved in distilled water and is mixed with mixing salt solution, is separately NaOH and the anhydrous Na of 2 ︰ 1 by mol ratio
2cO
3mixing is dissolved in distilled water and is made into mixed ammonium/alkali solutions;
Step 2: dropwise join in the reaction vessel of vigorous stirring while of being mixed ammonium/alkali solutions and the mixing salt solution of 1.7 ︰ 1 by volume ratio, slurries constant temperature 65 DEG C in reaction vessel is kept in dropping process, in dropping process maintenance reactor, slurry pH value is 9.8 ~ 10.3, after dropwising, continue constant temperature and stir 1h, make its abundant hybrid reaction;
Step 3: by reacted slurries at 65 DEG C of Water Under bath ageing 10h;
Step 4: resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain zinc-aluminium layered double hydroxide sample (2. number).
This zinc-aluminium layered double hydroxide sample (2. number), for except algae, when material dosage is 30mg/L, is 4.31 × 10 to plan post spore algae density
8after the water sample of individual/L processes, the clearance of chlorophyll a is more than 89.25%.
embodiment 3:
Step 1: the Mg (NO by mol ratio being 3 ︰ 1
3)
26H
2o and Al (NO
3)
39H
2o mixing is dissolved in distilled water and is mixed with mixing salt solution, is separately NaOH and the anhydrous Na of 3 ︰ 1 by mol ratio
2cO
3mixing is dissolved in distilled water and is made into mixed ammonium/alkali solutions;
Step 2: dropwise join in the reaction vessel of vigorous stirring while of being mixed ammonium/alkali solutions and the mixing salt solution of 1.2 ︰ 1 by volume ratio, slurries constant temperature 80 DEG C in reaction vessel is kept in dropping process, in dropping process maintenance reactor, slurry pH value is 9.8 ~ 10.3, after dropwising, continue constant temperature and stir 1h, make its abundant hybrid reaction;
Step 3: by reacted slurries at 70 DEG C of Water Under bath ageing 16h;
Step 4: resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain magnalium laminar double-metal hydroxide material.
This magnalium laminar double-metal hydroxide material is used for except algae, when material dosage is 30mg/L, is 4.68 × 10 to plan post spore algae density
8after the water sample of individual/L processes, the clearance of chlorophyll a is more than 83.33%.
embodiment 4:
Step 1: the Cu (NO by two trivalent metal ion mol ratios being 3 ︰ 1
3)
23H
2o, ZnSO
47H
2o and Al (NO
3)
39H
2o mixing is dissolved in distilled water and is mixed with mixing salt solution, is separately NaOH and the anhydrous Na of 3 ︰ 1 by mol ratio
2cO
3mixing is dissolved in distilled water and is made into mixed ammonium/alkali solutions;
Step 2: dropwise join in the reaction vessel of vigorous stirring while of being mixed ammonium/alkali solutions and the mixing salt solution of 1.1 ︰ 1 by volume ratio, slurries constant temperature 85 DEG C in reaction vessel is kept in dropping process, in dropping process maintenance reactor, slurry pH value is in 9.8 ~ 10.3 scopes, after dropwising, continue constant temperature and stir 1h, make its abundant hybrid reaction;
Step 3: by reacted slurries at 50 DEG C of Water Under bath ageing 16h;
Step 4: resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain copper zinc-aluminium layered double hydroxide sample.
This copper zinc-aluminium layered double hydroxide sample is used for except algae, when material dosage is 30mg/L, is 4.68 × 10 to plan post spore algae density
8after the water sample of individual/L processes, the clearance of chlorophyll a is more than 82.22%.
Claims (5)
1. a preparation method for layered double hydroxide wawter bloom algae remover, is characterized in that comprising the following steps:
(1) by mol ratio M
2+/ M
3+be that the soluble divalent metal salt of 2 ~ 3.5 ︰ 1 and trivalent metal salt are dissolved in distilled water and are mixed with mixing salt solution, by mol ratio OH
-/ CO
3 2-be NaOH and the anhydrous Na of 2 ~ 3 ︰ 1
2cO
3be dissolved in distilled water and be mixed with mixed ammonium/alkali solutions;
(2) be that the mixed ammonium/alkali solutions of 1.8 ~ 1 ︰ 1 and mixing salt solution dropwise join in the reaction vessel of vigorous stirring simultaneously by volume ratio, keep slurry temperature in reaction vessel constant in 65 ~ 85 DEG C in dropping process, in dropping process maintenance reactor, slurry pH value is in 9.8 ~ 10.3 scopes, after dropwising, continue constant temperature and stir 1h, make abundant hybrid reaction;
(3) reacted slurries are bathed ageing 6 ~ 16h at 50 ~ 70 DEG C of Water Unders;
(4) resultant is washed to neutrality, 80 DEG C of dryings, sieve, and obtain layered double hydroxide powder.
2. preparation method as claimed in claim 1, is characterized in that: in step (1), soluble divalent metal salt is ZnSO
47H
2o, Mg (NO
3)
26H
2o or Cu (NO
3)
23H
2o; Soluble trivalent metal salt is Al (NO
3)
39H
2o.
3. preparation method as claimed in claim 1, it is characterized in that: the layered double hydroxide powder that step (4) obtains, interlamellar spacing is 0.758nm, and powder size is 20 ~ 50 μm.
4. layered double hydroxide wawter bloom algae remover according to claim 1 is applied to wawter bloom except an algae, and from water, algae is removed in flocculation.
5. layered double hydroxide wawter bloom algae remover application as claimed in claim 4, it is characterized in that: first in water, add 20 ~ 30mg/L layered double hydroxide, then rapid stirring mixing 3min under 250r/min condition, low rate mixing 10 min under 30r/min condition again, last quiet heavy 10min, the algae flco natural sedimentation of generation.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106819755A (en) * | 2017-02-17 | 2017-06-13 | 内江师范学院 | A kind of reagent and method of turbidity removal of being taken away the puckery taste for fruit juice |
| CN106819755B (en) * | 2017-02-17 | 2020-10-16 | 内江师范学院 | Reagent and method for removing astringency and turbidity of fruit juice |
| CN110078186A (en) * | 2019-05-17 | 2019-08-02 | 上海大学 | A kind of dual-functional nanometer removes the preparation method and application of algae material |
| CN112028190A (en) * | 2020-08-24 | 2020-12-04 | 江南大学 | Method for preventing cyanobacterial bloom formation by blue membrane and zinc element cooperation |
| CN112551747A (en) * | 2020-12-02 | 2021-03-26 | 华南理工大学 | Double-metal hydroxide flocculating agent and method for treating wastewater containing nano plastic |
| CN114314780A (en) * | 2021-12-08 | 2022-04-12 | 重庆大学 | Application of diatomite-loaded magnetic nickel-iron layered double hydroxide as blue algae flocculant |
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Application publication date: 20150513 |