AU2017414238B2 - Method for enhancing algae coagulation using nitrogen-doped titanium dioxide and degrading algae-containing sediment in visible light simultaneously - Google Patents
Method for enhancing algae coagulation using nitrogen-doped titanium dioxide and degrading algae-containing sediment in visible light simultaneously Download PDFInfo
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- 230000015271 coagulation Effects 0.000 title claims abstract description 62
- 238000005345 coagulation Methods 0.000 title claims abstract description 62
- 241000195493 Cryptophyta Species 0.000 title claims abstract description 59
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000000593 degrading effect Effects 0.000 title abstract description 5
- 230000002708 enhancing effect Effects 0.000 title abstract description 4
- 239000013049 sediment Substances 0.000 title abstract 2
- 239000004408 titanium dioxide Substances 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000701 coagulant Substances 0.000 claims abstract description 37
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000010802 sludge Substances 0.000 claims description 49
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 41
- 238000011282 treatment Methods 0.000 claims description 35
- 239000006228 supernatant Substances 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 30
- 238000004062 sedimentation Methods 0.000 claims description 30
- 230000008569 process Effects 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract 1
- 241000192710 Microcystis aeruginosa Species 0.000 description 42
- 239000000243 solution Substances 0.000 description 24
- 230000015556 catabolic process Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 238000005286 illumination Methods 0.000 description 9
- 241000192700 Cyanobacteria Species 0.000 description 7
- 108010049746 Microcystins Proteins 0.000 description 7
- SRUWWOSWHXIIIA-UKPGNTDSSA-N Cyanoginosin Chemical compound N1C(=O)[C@H](CCCN=C(N)N)NC(=O)[C@@H](C)[C@H](C(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](C)NC(=O)C(=C)N(C)C(=O)CC[C@H](C(O)=O)N(C)C(=O)[C@@H](C)[C@@H]1\C=C\C(\C)=C\[C@H](C)[C@@H](O)CC1=CC=CC=C1 SRUWWOSWHXIIIA-UKPGNTDSSA-N 0.000 description 6
- 108010067094 microcystin Proteins 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- 230000015572 biosynthetic process Effects 0.000 description 2
- ATNHDLDRLWWWCB-AENOIHSZSA-M chlorophyll a Chemical compound C1([C@@H](C(=O)OC)C(=O)C2=C3C)=C2N2C3=CC(C(CC)=C3C)=[N+]4C3=CC3=C(C=C)C(C)=C5N3[Mg-2]42[N+]2=C1[C@@H](CCC(=O)OC\C=C(/C)CCC[C@H](C)CCC[C@H](C)CCCC(C)C)[C@H](C)C2=C5 ATNHDLDRLWWWCB-AENOIHSZSA-M 0.000 description 2
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- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 238000009360 aquaculture Methods 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229930002875 chlorophyll Natural products 0.000 description 1
- 235000019804 chlorophyll Nutrition 0.000 description 1
- 229930002868 chlorophyll a Natural products 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
Abstract
A method for enhancing algae coagulation using nitrogen-doped titanium dioxide and degrading algae-containing sediment in visible light simultaneously, comprising: (1) adding an algae-removing coagulant to the algae-containing water for stirring to complete coagulation, the algae-removing coagulant consisting of 50-400 parts by weight of N-TiO
Description
WVO2018/204lI9I87I4 VDVI AtVVIIIDI~~DlDIIIIIDD~I
M- dF;,ra* RV ~2 1 *(3))
(57~~~~f A 4NTt&i~ltt,~~() [PJ
t*fmZ(2): ql~~{tL~~ ~F;3: tL
APPLICATION OF N-TIO2 TO ENHANCE ALGAL COAGULATION AND
Technical Field
The present invention relates to a drinking water treatment process: in particular to
a method for enhancing algal coagulation and meanwhile degrading algae-containing
sludge under visible-light irradiation by the application of N-TiO 2
Background
In recent years the eutrophication of freshwater has occurred frequently
worldwide, including in China, leading to the proliferation of algae and the formation
of algal blooms, which seriously degrades the quality of raw water. The large-scale
growth of algae changes the physical and chemical characteristics of the water body,
inducing reductions of transparency and dissolved oxygen, and emission of odours. It
not only affects the aquaculture ecosystem, water supply, tourism, and ecological
landscape, but also seriously influences the daily life of human beings.
In drinking water treatment, the removal of algae mainly depends on the
coagulation process. However, since the algae are buoyant, the algal flocs formed
cannot easily settle, thereby reducing the algal removal efficiency and increasing the
burden on subsequent treatment processes. In addition, there are some species of
harmful algae, such as Microcystis aeruginosa (M. aeruginosa), that can release
microcystins and pose threats to public health. Through coagulation, these harmful algae will be transferred into the sludge and may cause secondary pollution. Therefore, the question of how to enhance the algal removal efficiency while also allowing the algae-containing sludge to be harmlessly discharged is an urgent problem to be solved.
Any discussion of the prior art throughout the specification should in no way be considered
as an admission that such prior art is widely known or forms part of common general
knowledge in the field.
Unless the context clearly requires otherwise, throughout the description and the claims, the
words "comprise", "comprising", and the like are to be construed in an inclusive sense as
opposed to an exclusive or exhaustive sense; that is to say, in the sense of "including, but not
limited to".
It is an object of the present invention to overcome or ameliorate at least one of the
disadvantages of the prior art, or to provide a useful alternative.
Summary
The present invention relates to the problems of low efficiency of removing algae and
secondary pollution caused by the algae-containing sludge.
According to a first aspect, the present invention provides a method for simultaneously
treating algae in raw water and sludge, the method comprising the following steps:
step 1): adding algae-removing coagulant to algae-containing raw water for coagulation,
wherein
the algae-removing coagulant is composed of the following components by mass:
to 400 parts of N-TiO 2 powder and 7.5 parts of polyaluminium ferric chloride
step 2): after sedimentation, algal flocs completely settle and algal cells in the supernatant are efficiently removed; step 3): separating off the supernatant, the remaining algae-containing sludge is stirred and irradiated under visible light, after treatment, the algal cells and cyanotoxins in sludge can be efficiently degraded.
The present invention provides a method for simultaneously treating algae in raw water and
sludge. The detailed steps are shown below:
Step 1): Adding the algae-removing coagulant to the algae-containing raw water for
coagulation;
the algae-removing coagulant is composed of the following components by mass:
50 to 400 parts of N-TiO 2 powder and 7.5 parts of polyaluminium ferric chloride
Step 2): After sedimentation, the algal flocs completely settle and the algal cells in the
supernatant are efficiently removed.
Step 3): After separating off the supernatant, the remaining algae-containing sludge is
stirred and irradiated under visible light. After hours or days of treatment, the algal cells and
cyanotoxins in the sludge can be efficiently degraded.
2a
The N-TiO2 is prepared as follows: 12 to 18 parts of tetrabutyl orthotitanate, 18 to
22 parts of ethyl alcohol, 28 to 35 parts of dilute nitric acid, and 0.05 to 0.5 parts of
urea by mass are mixed. After heating at 80 to 100 C for 3 to 5 hours and calcining at
400 to 500 C for 3 to 5 hours, the white solid obtained is N-TiO 2
. The algae-removing coagulant is prepared by mixing the N-TiO 2 powder and
PAFC according to the proportions described above.
Compared with the prior art, the present invention has the following beneficial
effects:
In the present invention, in comparison to the application of PAFC alone, mixing
with N-TiO2 can reduce the required PAFC dose to 50% and meanwhile enhance the
algal removal efficiency. N-TiO2 powder has negligible impact on the environment
and will not cause secondary pollution. The reduction of the required coagulant dose
can also decrease the content of heavy metals in water, which is beneficial for
improving the water quality. After coagulation, the N-TiO2 powder in the algae
containing flocs settles into the sludge. Under visible-light irradiation practically algal
cells in the sludge are broken within 12 hours, and 85% of the released cyanotoxins
can be degraded after 48 hours' treatment. After treatment, the sludge biomass is
markedly decreased and the quality of water contained in the sludge is improved,
which is beneficial for safe discharge of the sludge and reuse of water recovered from
the sludge.
Brief Description of the Drawings
Preferred embodiments of the invention will now be described, by way of
example only, with reference to the accompanying drawings in which:
Figure 1 shows the effect of different doses of PAFC on algal removal.
Figure 2 shows the algal removal efficiencies for treatments by PAFC combined
with different doses of N-TiO 2 during coagulation.
Figure 3 shows the algal removal efficiencies for treatments by PAFC combined
with different doses of N-TiO 2 during floc sedimentation.
Figure 4 shows the changes in chlorophyll-a contents during the degradation of
algae-containing sludge under visible light for treatments by different doses of N
TiO 2 .
Figure 5 shows the changes in microcystin concentrations during the degradation
of algae-containing sludge under visible light for treatments by different doses of N
TiO 2 .
Description of the Embodiments
It should be noted that the following detailed description is illustrative and is
intended to provide a further description of the invention. All technical and scientific
terms used herein have the same meaning as commonly understood by professionals
in the field that this invention belongs to.
It is to be noted that the terms used herein are for the purpose of describing
particular embodiments and are not intended to limit the exemplary embodiments of
the invention. For the terms used herein, unless the context clearly indicates otherwise,
singular forms are also intended to include plural forms.
The materials and reagents used in the present invention are commercially
available unless otherwise specified.
In the present invention, the algal removal efficiency, the algal cell degradation
efficiency, and the microcystin degradation efficiency are calculated as follows:
Algal removal efficiency (%)= (OD 6 80A-OD 6 80B) x 100% / OD 6 8 0 A (1)
A = raw water; B = supernatant after sedimentation; OD 680 = optical densities of the
extracts at wavelengths of 680 nm
Algal cell degradation efficiency (%)= (Chlc- ChlD)X 100% /Chlc (2)
Chl = chlorophyll; C = before treatment; D = after treatment.
Microcystin degradation efficiency (%)= (MCsE-MCsF)X 100% /MCsE (3)
MCs = microcystins; E = before treatment; F = after treatment.
As described in the background, there are deficiencies in the method for removing
algae in drinking water treatment, and the intracellular organic matter released by
algal cells cannot be effectively degraded. In order to solve these problems, the
present invention provides a method that can simultaneously treat the algae in water
and sludge. The method includes the following steps:
Step 1):Adding the algae-removing coagulant to the algae-containing raw water
for coagulation;
the algae-removing coagulant is composed of the following parts by mass: 50 to
400 parts of N-TiO 2 powder and 7.5 parts of PAFC.
Step 2):After sedimentation, the algal flocs completely settle and the algal cells in
the supernatant are efficiently removed.
Step 3):After separating off the supernatant, the remaining algae-containing
sludge is stirred and irradiated under visible light. After 12 to 48 hours of treatment,
the algal cells and cyanotoxins in sludge can be efficiently degraded.
In step 1, the above-mentioned algae-removing coagulant in a preferred
embodiment of the present invention is composed of the following components by
mass: 200 to 250 parts of N-TiO 2 powder and 7.5 parts of PAFC.
In the most preferred embodiment of the present invention, the above-mentioned
algae-removing coagulant is composed of the following components by mass: 200
parts of N-TiO 2 powder and 7.5 parts of PAFC.
The N-TiO2 is prepared as follows: 12 to 18 parts of tetrabutyl orthotitanate, 18 to
22 parts of ethyl alcohol, 28 to 35 parts of dilute nitric acid, and 0.05 to 0.5 parts of
urea by mass are mixed. After heating at 80 to 100 C for 3 to 5 hours and calcining at
400 to 500 C for 3 to 5 hours, the white solid obtained is N-TiO 2 .
In order to improve the algal removal efficiency and algal cell degradation
efficiency, the N-TiO2 in a preferred embodiment is prepared by the following
method:
15 parts of tetrabutyl orthotitanate are added to 20 parts of ethyl alcohol by mass.
After stirring, solution A is obtained.
0.05 to 0.5 parts of urea are added to 30 parts of dilute nitric acid. After stirring,
solution B is obtained.
Solution A is slowly added to solution B while stirring, and the pH is adjusted to a
value of 7 through the addition of a sodium hydroxide solution, and then the mixed
solution is heated at 80 C for 3 hours.
Thereafter, the mixed solution is centrifuged and the supernatant is discarded. The
remaining precipitate is washed with distilled water 3 times, and then calcined at
400 C to 500 C for 3 hours. The white powder obtained is N-TiO 2
. The particle size of the N-TiO 2 powder mentioned above is 50 to 150 mesh; more
preferably, the particle size of N-TiO 2 powder is 100 mesh.
In a preferred embodiment of the present invention, the algae-removing coagulant
is prepared by mixing the N-TiO 2 powder and PAFC according to the preferred
proportions described above.
Wherein, in step 1, the density of algae in raw water is 105 to 107 cells/mL. In the
coagulation process, the raw water is stirred at 150 to 250 rpm for 1 to 2 minutes, and
then stirred at 30 to 60 rpm for 10 to 20 minutes.
In the algae-removing coagulant, the required PAFC dose is 7.5 mg/L and the
required N-TiO2 dose is 50 to 400 mg/L. Without adding N-TiO 2 , the optimal
coagulation dose of PAFC for algal removal is 15 mg/L. After the algae-removing
coagulant is added to the algae-containing raw water, the small flocs are rapidly
formed during the rapid-stirring period. In this process, intense turbulence is
generated and the turbidity of water increases. During the slow stirring period, with
appropriate turbulence and sufficient sedimentation time (10 to 20 minutes), the flocs
gradually become large and can completely settle after coagulation based on the action of gravity. During the coagulation process, the OD6 8 0 value of the supernatant
(2 cm below the surface) is measured to monitor the removal of algal flocs.
In step 2, the sedimentation time is 10 to 60 minutes. During the sedimentation
period, the small flocs can be transferred to big flocs through collision, and then the
big flocs settle at the bottom to make the supernatant clean. At the end of
sedimentation, the turbidity of supernatant remains stable. The time required for flocs
to completely settle at the bottom can be determined by the OD6 8 0 value of the
supernatant during the sedimentation process.
Due to the algal cells' buoyancy, the high concentration of cells, and the high
negative charge on the surface of algal cells, the algal flocs produced by conventional
coagulants cannot efficiently settle, seriously decreasing the algal removal efficiency.
When appropriate doses of PAFC and N-TiO 2 powder are applied in coagulation, the
N-TiO2 powder can be incorporated into algal flocs to increase the flocs' size and
density. Combining the functions of PAFC and N-TiO 2 in algal coagulation, the flocs
that form can rapidly settle, which increases the algal removal efficiency.
In step 3, the volume of the discarded supernatant accounts for 93% to 97% of the
total volume of the algal suspension, the light intensity is 3000 to 15000 lux and the
stirring speed is 200 to 800 rpm.
Due to the advantages of non-toxicity, low cost, stable performance and corrosion
resistance, TiO2 is one of the most widely used photocatalysts. However, TiO 2 also
has some limitations: due to the large band gap (3.2 eV) and narrow range of light
absorption (mainly in the ultraviolet region), TiO2 has a low efficiency of solar light
utilization and quantum yield, and a high rate of semiconductor carrier recombination.
But when incorporating the element N (nitrogen) into the structure of TiO 2 (N-TiO 2 ),
the range of light wavelengths absorbed can be enlarged so as to increase the
photocatalytic activity under visible-light irradiation. Thus, N-TiO 2 can efficiently
disrupt algal cells and degrade the released cyanotoxins and organic matter under
visible light.
When the initial algal cells' density is 105 to 107 cells/mL, the algal removal
efficiency can be above 96% by adding 50 to 400 mg/L N-TiO 2 and 7.5mg/L PAFC in
the coagulation process. In the process of degrading algae-containing sludge, all algal
cells are broken within 12 hours' treatment. 85% of the total cyanotoxins are degraded
after 48 hours' treatment.
In order to help professionals in the relevant fields to understand the present
invention more thoroughly, specific embodiments and contrastive examples are
described below.
Embodiment 1
The algae-removing coagulant consists of the following components: 50 parts of
N-TiO2 powder (100 mesh) and 7.5 parts of PAFC by mass.
M. aeruginosa is used as the model alga in this embodiment to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa concentration is diluted with deionized water to xI106 cells/mL M. aeruginosa solution to obtain the algae-containing raw water. After 7.5 mg PAFC and 50 mg N
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1
min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both
the coagulation and the sedimentation processes. Samples collected from 2 cm below
the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. The algal removal efficiency reaches a maximum at 1 h after the
completion of coagulation, which is 96% (Figures 2 and 3).
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 48 hours' treatment,
41.6% of algal cells are broken while some microcystins still remain intracellularly
(Figures 4 and 5).
Embodiment 2
The algae-removing coagulant consists of the following components: 100 parts of
N-TiO2 powder (100 mesh) and 7.5 parts of PAFC by mass.
Maeruginosa is used as the model alga in this embodiment to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M.aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to xI106 cells/mL M. aeruginosa solution to obtain the algae-containing raw water. After 7.5 mg PAFC and 100 mg N
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1
min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both
the coagulation and the sedimentation processes. Samples collected from 2 cm below
the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. The algal removal efficiency reaches a maximum at 1 h after the
completion of coagulation, which is 97% (Figures 2 and 3).
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 48 hours' treatment,
59.9% of algal cells are disrupted while some microcystins still remain intracellularly
(Figures 4 and 5).
Embodiment 3
The algae-removing coagulant consists of the following components: 200 parts of
N-TiO2 powder (100 mesh) and 7.5 parts of PAFC by mass.
Maeruginosa is used as the model alga in this embodiment to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to 1x106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFC and 200 mg N
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1
min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both
the coagulation and the sedimentation processes. Samples collected from 2 cm below
the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. The algal removal efficiency reaches a maximum at 10 min after the
completion of coagulation, which is 98% (Figures 2 and 3).
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 12 hours' treatment,
all algal cells are broken, and after 48 hours' treatment the efficiency of microcystin
degradation is 84.2% (Figures 4 and 5).
Embodiment 4
The algae-removing coagulant consists of the following components: 400 parts of
N-TiO2 powder (100 mesh) and 7.5 parts of PAFC by mass.
Maeruginosa is used as the model alga in this embodiment to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to 1x106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFC and 400 mg N
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1 min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both the coagulation and the sedimentation processes. Samples collected from 2 cm below the surface are characterised by OD 6 8 0 to calculate the algal cell density in the supernatant. The algal removal efficiency reaches a maximum at 10 min after the completion of coagulation, which is 98% (Figures 2 and 3).
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 12 hours' treatment,
all algal cells are broken, and after 48 hours' treatment the efficiency of microcystin
degradation is 87.6% (Figures 4 and 5).
Among embodiments 1 to 4, the algae-removing coagulant in embodiment 3 is
preferred. In Embodiments 1 and 2, the algal cells and cyanotoxins in sludge cannot
be effectively degraded within 48 hours. In Embodiment 4, the dose of N-TiO 2 is
excessive and some of the added N-TiO 2 will remain in the supernatant after
coagulation, which will decrease the water quality and increase the treatment cost.
In order to increase the algal removal efficiency and decrease the required
coagulant dose while efficiently degrading algae-containing sludge, the present
invention combines and optimizes the photocatalysts and conventional coagulants to
simultaneously enhance algal coagulation and degrade the algae-containing sludge.
Through screening different types of photocatalysts, N-TiO2 is chosen as the preferred
photocatalyst in the present invention. Compared with the coagulation function of
PAFC, N-TiO2 powder can serve as the core of algal flocs during the coagulation
process, which can increase the flocs' density, thereby enhancing the algal
coagulation and sedimentation and solving the issues caused by the buoyancy of algal cells. In addition, N-TiO2 can effectively disrupt algal cells and degrade the cyanotoxins and organic matter under visible light.
Based on the characteristics of algae, PAFC is chosen as the preferred coagulant
in the present invention. It combines the advantages of Al and Fe salts, and has a
significant improvement in the morphology of Al and Fe ions. PAFC combined with
N-TiO2 has the best results for the treatment of algae-containing raw water. For the
optimization of dosages, the optimum dose of PAFC is 7.5 parts by mass. Combining
with the optimum dose of N-TiO 2 (best treatment results with the lowest dose), the
algal removal efficiency will decrease when the dose of PAFC exceeds 7.5 parts by
mass. When the dose of PAFC is less than 7.5 parts by mass, the algal removal
efficiency cannot reach the optimum. Preferably, doses of 7.5 parts of PAFC and 50
to 400 parts of N-TiO 2 powder are selected.
It is found that different types and doses of coagulants and photocatalysts have
various results for the treatment of algae in raw water. Thus, Contrastive Examples 1
to 5 are shown below, but the research is not limited to the following contrastive
examples.
Contrastive Example 1
The algae-removing coagulant consists of the following component: 7.5 parts of
M. aeruginosais used as the model alga in this example to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to xi106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFC is added, the M.
aeruginosa solution is stirred at 250 rpm for 1 min and 30 rpm for another 30 min.
Algal removal efficiencies are measured for both the coagulation and the
sedimentation processes. Samples collected from 2 cm below the surface are
characterised by OD 6 8 0to calculate the algal cell density in the supernatant. Results
show that the rate of floc formation is slow and the algal removal efficiency during
coagulation is only 5 to 6% (Figure 2). Besides that, when settling for 30 minutes
after coagulation the algal removal efficiency is only 60%, and after 120 minutes'
sedimentation the algal removal efficiency reaches the maximum of just 80% (Figure
3).
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After treatment, algal
cells cannot be effectively broken and the microcystin degradation efficiency is
negligible (Figures 4 and 5).
In Figure 1, it can be seen that when using PAFC only, the algal removal
efficiency of 7.5 mg/L PAFC is just 60%. As the dose of PAFC increases to 15 mg/L,
the algal removal efficiency is 90%, which is the maximum value.
Contrastive Example 2
The algae-removing coagulant consists of the following components: 200 parts of
N-TiO2 (100 mesh) and 7.5 parts of poly-aluminium-ferric-silicate-chloride(PAFSC)
by mass.
M. aeruginosa is used as the model alga in this example to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to xi106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFSC and 200 mg
N-TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for
1 min and 30 rpm for another 30 min. Algal removal efficiencies are measured for
both the coagulation and the sedimentation processes. Samples collected from 2 cm
below the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. When settling for 30 minutes after coagulation, the algal removal
efficiency is 80%.
Contrastive Example 3
The algae-removing coagulant consists of the following components: 200 parts of
TiO2 powder (100 mesh) and 7.5 parts of PAFC by mass.
M. aeruginosa is used as the model alga in this example to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 T) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
1L beakers each containing 1L of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to lx106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFC and 200 mg
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1
min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both
the coagulation and the sedimentation process. Samples collected from 2 cm below
the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. When settling for 30 minutes after coagulation, the algal removal
efficiency is 85%.
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 48 hours' treatment,
49% of algal cells are broken and 48.4% of the microcystins are degraded.
Contrastive Example 4
The algae-removing coagulant consists of the following components: 200 parts of
rare-earth-element-doped TiO2 (100 mesh) and 7.5 parts of PAFSC by mass.
The rare-earth-element-doped TiO 2 is prepared as follows. Tetrabutyl
orthotitanate is added to 20 mL ethyl alcohol. After 2 hours' stirring, lanthanum
nitrate is added and a sol-gel is formed. Then the sol-gel is dried and calcined at
400 C for 5 h to obtain the rare-earth-element-doped TiO 2 .
M. aeruginosa is used as the model alga in this example to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 'C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of
IL beakers each containing IL of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to xi106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 7.5 mg PAFSC and 200 mg
rare-earth-element-doped TiO2 are simultaneously added, the M. aeruginosa solution
is stirred at 250 rpm for 1 min and 30 rpm for another 30 min. Algal removal
efficiencies are measured for both the coagulation and the sedimentation processes.
Samples collected from 2 cm below the surface are characterised by OD6 8 0 to
calculate the algal cell density in the supernatant. When settling for 30 minutes after
coagulation, the algal removal efficiency is 83%.
After coagulation and sedimentation, 930 mL of supernatant is removed, leaving
mL of lab-simulated cyanobacteria-containing sludge. The sludge is magnetically
stirred at 500 rpm under visible-light irradiation (8000 lux). After 48 hours' treatment,
43% of algal cells are broken and 45.6% of the microcystins are degraded.
Contrastive Example 5
The algae-removing coagulant consists of the following components: 200 parts of
N-TiO2 (100 mesh) and 10 parts of PAFC by mass.
M. aeruginosa is used as the model alga in this example to prepare the algae
containing raw water. This strain is grown in BG11 medium at constant temperature
(25 C) with a light/dark cycle (12h/12h) under 2000 lux illumination. The cultures
are harvested at the exponential phase of growth.
The coagulation experiments are performed with a six-paddle stirrer in a series of IL
beakers each containing 1L of M. aeruginosa culture. The initial M. aeruginosa
concentration is diluted with deionized water to 1x106 cells/mL M. aeruginosa
solution to obtain the algae-containing raw water. After 10 mg PAFC and 200 mg N
TiO2 are simultaneously added, the M. aeruginosa solution is stirred at 250 rpm for 1
min and 30 rpm for another 30 min. Algal removal efficiencies are measured for both
the coagulation and the sedimentation processes. Samples collected from 2 cm below
the surface are characterised by OD 6 8 0 to calculate the algal cell density in the
supernatant. When settling for 30 minutes after coagulation, the algal removal
efficiency is 90%.
In summary, the algae-removing coagulant described in the present invention is
PAFC mixed with N-TiO 2 powder. Compared with applying PAFC only, adding N
TiO2 can reduce the required PAFC dosage by 50% and increase the algal removal
efficiency to 96%, and the results are better than those obtained in contrastive
examples to 5. The N-TiO 2 powder has little impact on the environment and will not
cause secondary pollution. After coagulation, the N-TiO2 powder settles into the
sludge with the algal flocs. With the algae-containing sludge being treated by visible
light irradiation while stirring, all algal cells can be disrupted within 12 hours, and
more than 85% of the cyanotoxins can be degraded after 48 hours' treatment. Results
are better than those of contrastive examples 1 to 5. After treatment, the sludge
biomass is reduced, which can increase the quality of water contained in the sludge,
which is beneficial for the reuse or discharge of sludge. In addition, the proportion of components in the algae-removing coagulant of the present invention is also very critical. When changing the proportion of components, the algal removal efficiency and sludge treating efficiency will be markedly decreased.
The above embodiments are preferred ones in the present invention, and the
present invention is not limited by the above embodiments. Any changes,
modifications, substitutions, combinations, and simplifications are included in the
scope of the present invention.
Claims (5)
1. A method for simultaneously treating algae in raw water and sludge, the
method comprising the following steps:
step 1): adding algae-removing coagulant to algae-containing raw water for
coagulation, wherein
the algae-removing coagulant is composed of the following components by mass:
to 400 parts of N-TiO 2 powder and 7.5 parts of polyaluminium ferric chloride
(PAFC);
step 2): after sedimentation, algal flocs completely settle and algal cells in the
supernatant are efficiently removed;
step 3): separating off the supernatant, the remaining algae-containing sludge is
stirred and irradiated under visible light, after treatment, the algal cells and
cyanotoxins in sludge can be efficiently degraded.
2. The method according to claim 1, wherein the algae-removing coagulant in step
1 is composed of the following components by mass: 200 to 250 parts of N-TiO 2
powder and 7.5 parts of PAFC.
3. The method according to claim 2, wherein the algae-removing coagulant is
composed of the following components by mass: 200 parts of N-TiO 2 powder and 7.5
parts of PAFC.
4. The method according to claim 1, wherein the N-TiO2 in step 1 is prepared as
follows: 12 to 18 parts of tetrabutyl orthotitanate, 18 to 22 parts of ethyl alcohol, 28 to
parts of dilute nitric acid, and 0.05 to 0.5 parts of urea by mass are mixed; after heating at 80 to 100 T for 3 to 5 hours and calcining at 400 to 500 T for 3 to 5 hours, the white solid obtained is N-TiO 2
. 5. The method according to claim 4, wherein the size of N-TiO 2 powder is 50 to
500 mesh and the preferred size of N-TiO 2 powder is 100 mesh.
6. The method according to claim 1, wherein the algae-removing coagulant in step
1 is prepared by mixing the N-TiO 2 powder and PAFC according to the preferred
proportions.
7. The method according to claim 1, wherein, in step 1, the density of algae in raw
water is 105 to 107 cells/mL and the raw water is stirred at 150 to 250 rpm for 1 to 2
minutes, and then stirred at 30 to 60 rpm for 10 to 20 minutes duringthe coagulation
process.
8. The method according to claim 7, wherein, in step 1, the dose of PAFC added
to raw water is 7.
5 mg/L and the dose of N-TiO 2 added to raw water is 50 to 400
mg/L.
9. The method according to claim 1, wherein the sedimentation time in step 2 is
to 60 minutes.
10. The method according to claim 1, wherein, in step 3, the volume of the
discarded supernatant occupies 93% to 97% of the total volume of the algal
suspension, the light intensity is 3000 to 15000 lux, and the stirring speed is 200 to
800 rpm.
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| CN201710352078.3A CN107140719B (en) | 2017-05-18 | 2017-05-18 | Method for strengthening algae coagulation by using nitrogen-doped titanium dioxide and simultaneously degrading algae-containing sediment under visible light |
| PCT/CN2017/104482 WO2018209874A1 (en) | 2017-05-18 | 2017-09-29 | Method for enhancing algae coagulation using nitrogen-doped titanium dioxide and degrading algae-containing sediment in visible light simultaneously |
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| CN107098453B (en) * | 2017-05-18 | 2020-05-12 | 山东大学 | Algae removal coagulant for strengthening algae coagulation and simultaneously degrading algae-containing sediment under visible light, and preparation method and application thereof |
| CN107140719B (en) * | 2017-05-18 | 2020-05-08 | 山东大学 | Method for strengthening algae coagulation by using nitrogen-doped titanium dioxide and simultaneously degrading algae-containing sediment under visible light |
| CN107570197A (en) * | 2017-10-11 | 2018-01-12 | 南开大学 | A kind of synthetic method of hollow auto-dope structure bimetallic photochemical catalyst and application |
| CN108147496B (en) * | 2017-12-21 | 2020-06-05 | 山东大学 | Method for degrading water pollutants by using nano photocatalyst flocs |
| CN107935269B (en) * | 2017-12-21 | 2020-05-12 | 山东大学 | Water treatment process capable of recycling coagulant and photocatalytic material and realizing zero discharge of muddy water |
| CN110354833B (en) * | 2019-06-18 | 2022-12-23 | 中冶华天工程技术有限公司 | Method for preparing visible light response mesoporous titanium dioxide material by utilizing coagulated sludge |
| CN113511712A (en) * | 2021-05-25 | 2021-10-19 | 中国人民解放军陆军勤务学院 | Application of titanium trichloride and treatment method of high algae-laden water containing copper green microcystis |
| CN114890524B (en) * | 2022-04-18 | 2023-07-25 | 武汉理工大学三亚科教创新园 | Algae removing agent based on amphiphilic dendrimer and algae removing method thereof |
| CN114956412A (en) * | 2022-07-08 | 2022-08-30 | 天津农学院 | Catalytic treatment process for microcystin in aquaculture tail water |
| CN117494290B8 (en) * | 2023-12-29 | 2024-06-04 | 深圳市大鹏园林生态建设有限公司 | Ecological garden greening optimization method |
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