CN109179796A - Absorption/flocculation/photocatalysis composite dye waste water treating agent and wastewater treatment method - Google Patents
Absorption/flocculation/photocatalysis composite dye waste water treating agent and wastewater treatment method Download PDFInfo
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- CN109179796A CN109179796A CN201811403788.5A CN201811403788A CN109179796A CN 109179796 A CN109179796 A CN 109179796A CN 201811403788 A CN201811403788 A CN 201811403788A CN 109179796 A CN109179796 A CN 109179796A
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- waste water
- wastewater treatment
- gadolinium
- cerium
- treatment agent
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 65
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 56
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 55
- 239000010919 dye waste Substances 0.000 title claims abstract description 27
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 21
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 21
- 230000016615 flocculation Effects 0.000 title claims abstract description 19
- 238000005189 flocculation Methods 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 14
- 239000000975 dye Substances 0.000 claims abstract description 75
- 239000002351 wastewater Substances 0.000 claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 43
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 42
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000012986 modification Methods 0.000 claims abstract description 25
- 230000004048 modification Effects 0.000 claims abstract description 25
- 238000012545 processing Methods 0.000 claims abstract description 13
- 229920000592 inorganic polymer Polymers 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 29
- 238000002360 preparation method Methods 0.000 claims description 27
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000007853 buffer solution Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 10
- 238000005286 illumination Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 229910052719 titanium Inorganic materials 0.000 claims description 8
- 239000010936 titanium Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 239000012736 aqueous medium Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 6
- XWFVFZQEDMDSET-UHFFFAOYSA-N gadolinium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Gd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XWFVFZQEDMDSET-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000000643 oven drying Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 2
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 12
- 238000011282 treatment Methods 0.000 abstract description 8
- 238000004042 decolorization Methods 0.000 abstract description 6
- 230000000593 degrading effect Effects 0.000 abstract description 4
- 230000009102 absorption Effects 0.000 abstract description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- 239000004411 aluminium Substances 0.000 description 7
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 239000000126 substance Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000005909 Kieselgur Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000013505 freshwater Substances 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The present invention provides a kind of absorption/flocculation/photocatalysis composite dye waste water treating agent and wastewater treatment methods, are related to technical field of waste water processing；Absorption/the flocculation/photocatalysis composite dye waste water treating agent is made of raw material from the following weight: cerium and gadolinium co-doped nano TiO20.1-0.5 parts, 60-80 parts of PDMDAAC modification infusorial earth, 20-35 parts of inorganic polymer flocculant.Absorption, flocculation, photocatalysis are combined by the present invention, and select suitable raw material, keep waste water treating agent obtained excellent to the treatment effect of waste water from dyestuff, and percent of decolourization, COD removal rate are high, good degrading effect.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular at a kind of absorption/flocculation/photocatalysis composite dye waste water
Manage agent and wastewater treatment method.
Background technique
Water is the Source of life of the mankind, animal, plant, and having left the water mankind will not exist, and the life of water is needed on the earth
Object cannot also survive.It is main dirty since a large amount of freshwater resources reduce global freshwater resources year by year by environmental pollution
There are untreated or part processing city domestic sewage, toxic industrial waste water, the discharge of harmful wastewater from chemical industry and by agriculture in dye source
The underground water of chemicals contamination.Dyestuff is one of pollution sources important in water pollution, be mainly derived from weaving, papermaking, plastics, food and
The discharge of wastewater of the companies such as cosmetics.Waste water from dyestuff pours in China's water body environment, it has also become threatens China's water environment safety
An important factor for.The characteristics of waste water from dyestuff may be summarized to be " three big one is difficult ": wastewater flow rate is big, toxicity is big, pollution is big and difficult.
In view of the water body dye discoloration situation of current sternness, develop low power consuming, high efficiency, dyestuff environmentally protective, applied widely
Polluted water body repairing method and technology have been to be concerned by more and more people.Treatment method of printing and dying wastewater has bioanalysis, electrification at present
Method, chemical oxidization method, flocculence and absorption method etc..
CN 105800757 discloses a kind of dye wastewater treatment agent, the dye wastewater treatment agent, by such as aluminium polychloride
Iron, bentonite, Sodium Polyacrylate, active carbon, visible light catalyst, distilled water are made.The production of the dye wastewater treatment agent is former
Expect from a wealth of sources, can effectively remove the organic dyestuff in water, processing organic dyestuff is thorough, processing cost is low, non-toxic, without dirt
Dye.But it is in the description, only demonstrating it has good effect to methylene blue dye wastewater, therefore not can determine that it
Whether there is good degradation effect to other waste water from dyestuff.For this purpose, developing one kind has excellent degradation to a variety of waste water from dyestuff
The waste water treating agent of effect has important research significance.Wherein diatomite, nano-TiO2It is to be answered in dye wastewater treatment
It with more adsorbent and photochemical catalyst, but does not have been reported that, is provided commonly for the two as main matter in the prior art
In the processing of waste water from dyestuff, and further, the property of the two is also required to advanced optimize.
After diatomite is ancient times unicellular rudimentary plant diatom remains accumulation, one kind for being formed by preliminary diagenesis
With porous biological silicalite.Diatomite is made of the wall shell of diatom, is had on wall shell multistage, a large amount of, ordered arrangement
Micropore.This unique structure assigns its many excellent performance: chemical property is stablized, and porosity is big, large specific surface area, absorption
Property is strong.Therefore application prospect of the diatomite in terms of dye wastewater treatment is very wide, but single diatomite handles dyestuff
The effect of waste water is not especially desirable.
In recent years, the environmentally friendly cry that the scarcity of China's water resource and dyeing grow to even greater heights makes techniques of Dyeing Wastewater Treatment
Gradually paid attention to by people.With nano-TiO2Photochemical catalyst is that the photocatalysis oxidation technique of representative is energy-efficient, dirty due to having
Dye object degrades the advantages that thorough and becomes the hot spot of wastewater processing technology research.But TiO2With biggish forbidden bandwidth, electronics
Transition only absorbs ultraviolet light.This makes nano-TiO2Photochemical catalyst is lower to the proportion of utilization of solar energy.Therefore, it is intended that passing through
The a small amount of suitable element of incorporation improves TiO2Photocatalytic activity and its utilization rate to sunlight.It is special that rare earth metal has
Outermost electron structure, easily dispersion and unreducible characteristic, have been increasingly becoming the emphasis of doping system research.
Summary of the invention
The purpose of the present invention is to provide a kind of absorption/flocculation/photocatalysis composite dye waste water treating agent and wastewater treatments
Absorption, flocculation, photocatalysis are combined by method, and select suitable raw material, make waste water treating agent obtained to waste water from dyestuff
Treatment effect it is excellent, percent of decolourization, COD removal rate are high, good degrading effect.
In order to achieve the above object, the present invention is achieved by the following technical programs:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.1-0.5 parts；
60-80 parts of PDMDAAC modification infusorial earth；
20-35 parts of inorganic polymer flocculant.
Preferably, dye wastewater treatment agent is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.3 part；
72 parts of PDMDAAC modification infusorial earth；
26 parts of inorganic polymer flocculant.
The preparation method of dye wastewater treatment agent is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio
In, 20-30min, mixing speed 600-1200r/min are stirred at 50-60 DEG C.
In the present invention, inorganic polymer flocculant is one of aluminium polychloride, polyaluminium sulfate, bodied ferric sulfate.
Cerium and gadolinium co-doped nano TiO2Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 1.5-2.5 is made；By tetrafluoride
Titanium is dissolved in above-mentioned buffer solution, and 0.05molL is made-1Titanium tetrafluoride solution, adjust solution ph to 1.5-2；(the solution
Stablize, can store the long period.)
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added one
Quantitative gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 15-17h at 165 DEG C；
Centrifugation, is rinsed 3 times respectively with deionized water, dehydrated alcohol, and gained powder is dried 20-24h in 100 DEG C of vacuum ovens,
To obtain the final product.
Wherein, cerium and gadolinium co-doped nano TiO2In, cerium, gadolinium, titanium atomic ratio be 0.5-1.5:0.3-0.8:100.Into
One step preferably, cerium and gadolinium co-doped nano TiO2In, cerium, gadolinium, titanium atomic ratio be 1:0.5:100.
The preparation method of PDMDAAC modification infusorial earth the following steps are included:
(1) 60-100 mesh is crossed after grinding diatomite, and the powder for being attached to diatomite surface is washed away with distilled water, is placed in
Drying, takes out after 850 DEG C of calcination 1.5h of Muffle furnace, is cooled to room temperature in 70-80 DEG C of vacuum oven；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 30-40% and carry out acidleach processing,
Being washed repeatedly after suction filtration using water is neutrality to filtrate, then is placed in drying in 70-80 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite and PDMDAAC 1:0.02-0.045 in mass ratio
It closes, 2h is stirred to react at 65 DEG C, is then filtered, after being washed with water 3 times, be placed in drying in 70-80 DEG C of vacuum oven, i.e.,
?.
A kind of dye waste water treatment method, comprising the following steps:
The pH value of waste water from dyestuff is adjusted to 5.5-7, is placed under the irradiation of nature sunlight or under simulated solar irradiation irradiation, adds
Enter the dye wastewater treatment agent in the present invention, 40-50min is stirred to waste water, mixing speed 30-50r/min is stood later
10-15min, to treated, waste water is separated by solid-liquid separation, and the additional amount of the dye wastewater treatment agent is useless for dyestuff to be processed
The 0.2-0.7% of water weight.The intensity of illumination of the nature sunlight irradiation or simulated solar irradiation irradiation is in 15000LX or more.
The beneficial effects of the present invention are:
Waste water treating agent of the invention, based on PDMDAAC modification infusorial earth, what cooperation was prepared through ad hoc approach
Cerium and gadolinium co-doped nano TiO2And common inorganic polymer flocculant and cationic organic high-molecular in water treatment technology
Flocculant cooperates cerium and gadolinium co-doped nano TiO first with the stronger absorption property of PDMDAAC modification infusorial earth2Excellent
Photocatalysis effect, and act synergistically simultaneously with each flocculant, it can be achieved that waste water from dyestuff it is effective adsorb, photocatalysis and cohesion,
Good purified treatment can be played to waste water from dyestuff.
In the present invention, PDMDAAC modification infusorial earth is that diatomite is obtained through PDMDAAC modification；PDMDAAC molecule contains ratio
More positive charge neutralizes with the SiO- on surface in diatomite, and is adsorbed in diatomite surface, make modified diatomite at
For positively charged particle；By modification, increase the specific surface area of diatomite molecule, and increase cation exchange volume and
Surface property is changed, dramatically increases it to the absorption property of the pollutant in waste water from dyestuff.Inorganic polymer is combined at this time
Flocculant can form quickly absorption and flocculation to the tiny component in waste water, form biggish wadding aggressiveness, can effectively accelerate to give up
The flocculation of each substance in water, and be conducive to the separation of solid and liquid after wastewater treatment.
The cerium and gadolinium co-doped nano TiO being prepared2For hollow structure, which has specific surface area high, close
Spend the features such as low；And use Ce elements and gadolinium element to nano-TiO2Hollow sphere is doped, and can effectively widen its absorbing wavelength
Range, and further increase it than specific surface area, and high specific surface area makes the photocatalytic activity point for having more, at the same cerium and
Gadolinium has synergistic effect, greatly improves cerium and gadolinium co-doped nano TiO2Photocatalysis performance.
Absorption, flocculation, photocatalysis are combined by waste water from dyestuff of the present invention, and select suitable raw material, are made obtained useless
Water treatment agent is excellent to the treatment effect of waste water from dyestuff, and percent of decolourization, COD removal rate are high, good degrading effect.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.3 part；
72 parts of PDMDAAC modification infusorial earth；
26 parts of aluminium polychloride.
The preparation method of dye wastewater treatment agent is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio
In, 30min, mixing speed 800r/min are stirred at 55 DEG C.
Cerium and gadolinium co-doped nano TiO2Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 2 is made；Titanium tetrafluoride is dissolved in
Above-mentioned buffer solution, is made 0.05molL-1Titanium tetrafluoride solution, adjust solution ph to 2；
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added one
Quantitative gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 15h at 165 DEG C；From
The heart is rinsed 3 times respectively with deionized water, dehydrated alcohol, by gained powder in 100 DEG C of vacuum ovens it is dry for 24 hours to get.
The cerium and gadolinium co-doped nano TiO being prepared2In, cerium, gadolinium, titanium atomic ratio be 1:0.5:100.
The preparation method of PDMDAAC modification infusorial earth the following steps are included:
(1) it is sieved with 100 mesh sieve after grinding diatomite, the powder for being attached to diatomite surface is washed away with distilled water, is placed in 80
DEG C vacuum oven in drying, take out, be cooled to room temperature after 850 DEG C of calcination 1.5h of Muffle furnace；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 35% and carry out acidleach processing, filtered
Being washed repeatedly using water afterwards is neutrality to filtrate, then is placed in drying in 80 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite with PDMDAAC 1:0.035 in mass ratio, 65
Be stirred to react 2h at DEG C, then filter, after being washed with water 3 times, be placed in 80 DEG C of vacuum oven drying to get.
Embodiment 2:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.5 part；
68 parts of PDMDAAC modification infusorial earth；
35 parts of bodied ferric sulfate.
The preparation method of dye wastewater treatment agent is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio
In, 30min, mixing speed 600r/min are stirred at 50 DEG C.
Cerium and gadolinium co-doped nano TiO2Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 2.5 is made；Titanium tetrafluoride is molten
In above-mentioned buffer solution, 0.05molL is made-1Titanium tetrafluoride solution, adjust solution ph to 2；
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added one
Quantitative gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 17h at 165 DEG C；From
The heart is rinsed 3 times respectively with deionized water, dehydrated alcohol, by gained powder in 100 DEG C of vacuum ovens it is dry for 24 hours to get.
The cerium and gadolinium co-doped nano TiO being prepared2In, cerium, gadolinium, titanium atomic ratio be 1.5:0.5:100.
The preparation method of PDMDAAC modification infusorial earth the following steps are included:
(1) 60 meshes are crossed after grinding diatomite, and the powder for being attached to diatomite surface is washed away with distilled water, is placed in 75 DEG C
Vacuum oven in drying, take out, be cooled to room temperature after 850 DEG C of calcination 1.5h of Muffle furnace；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 40% and carry out acidleach processing, filtered
Being washed repeatedly using water afterwards is neutrality to filtrate, then is placed in drying in 75 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite with PDMDAAC 1:0.03 in mass ratio, 65
Be stirred to react 2h at DEG C, then filter, after being washed with water 3 times, be placed in 75 DEG C of vacuum oven drying to get.
Embodiment 3:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.4 part；
80 parts of PDMDAAC modification infusorial earth；
22 parts of polyaluminium sulfate.
The preparation method of dye wastewater treatment agent is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio
In, 25min, mixing speed 800r/min are stirred at 60 DEG C.
Cerium and gadolinium co-doped nano TiO2Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 1.5 is made；Titanium tetrafluoride is molten
In above-mentioned buffer solution, 0.05molL is made-1Titanium tetrafluoride solution, adjust solution ph to 2；
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added one
Quantitative gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 16h at 165 DEG C；From
The heart is rinsed 3 times respectively with deionized water, dehydrated alcohol, by gained powder in 100 DEG C of vacuum ovens it is dry for 24 hours to get.
The cerium and gadolinium co-doped nano TiO being prepared2In, cerium, gadolinium, titanium atomic ratio be 0.5:0.8:100.
The preparation method of PDMDAAC modification infusorial earth the following steps are included:
(1) 80 meshes are crossed after grinding diatomite, and the powder for being attached to diatomite surface is washed away with distilled water, is placed in 80 DEG C
Vacuum oven in drying, take out, be cooled to room temperature after 850 DEG C of calcination 1.5h of Muffle furnace；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 30% and carry out acidleach processing, filtered
Being washed repeatedly using water afterwards is neutrality to filtrate, then is placed in drying in 80 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite with PDMDAAC 1:0.02 in mass ratio, 65
Be stirred to react 2h at DEG C, then filter, after being washed with water 3 times, be placed in 80 DEG C of vacuum oven drying to get.
Embodiment 4:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, by being made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.1 part；
60 parts of PDMDAAC modification infusorial earth；
20 parts of aluminium polychloride.
The preparation method of dye wastewater treatment agent is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio
In, 20min, mixing speed 1200r/min are stirred at 55 DEG C.
Cerium and gadolinium co-doped nano TiO2Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 2 is made；Titanium tetrafluoride is dissolved in
Above-mentioned buffer solution, is made 0.05molL-1Titanium tetrafluoride solution, adjust solution ph to 1.5；
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added one
Quantitative gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 15h at 165 DEG C；From
The heart is rinsed 3 times respectively with deionized water, dehydrated alcohol, by gained powder in 100 DEG C of vacuum ovens dry 22h to get.
The cerium and gadolinium co-doped nano TiO being prepared2In, cerium, gadolinium, titanium atomic ratio be 1.2:0.4:100.
The preparation method of PDMDAAC modification infusorial earth the following steps are included:
(1) it is sieved with 100 mesh sieve after grinding diatomite, the powder for being attached to diatomite surface is washed away with distilled water, is placed in 70
DEG C vacuum oven in drying, take out, be cooled to room temperature after 850 DEG C of calcination 1.5h of Muffle furnace；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 33% and carry out acidleach processing, filtered
Being washed repeatedly using water afterwards is neutrality to filtrate, then is placed in drying in 70 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite with PDMDAAC 1:0.045 in mass ratio, 65
Be stirred to react 2h at DEG C, then filter, after being washed with water 3 times, be placed in 70 DEG C of vacuum oven drying to get.
Embodiment 5:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.4 part；
70 parts of PDMDAAC modification infusorial earth；
25 parts of aluminium polychloride.
Preparation method, cerium and the gadolinium co-doped nano TiO of dye wastewater treatment agent2Preparation method, PDMDAAC modified silicon
The preparation method of diatomaceous earth is the same as embodiment 1.
Embodiment 6:
A kind of absorption/flocculation/photocatalysis composite dye waste water treating agent, is made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.25 part；
65 parts of PDMDAAC modification infusorial earth；
30 parts of polyaluminium sulfate.
Preparation method, cerium and the gadolinium co-doped nano TiO of dye wastewater treatment agent2Preparation method, PDMDAAC modified silicon
The preparation method of diatomaceous earth is the same as embodiment 2.
Embodiment 7:
A kind of dye waste water treatment method, comprising the following steps:
The pH value of waste water from dyestuff is adjusted to 6.5, is placed under the irradiation of nature sunlight, is added in the embodiment of the present invention 1
Dye wastewater treatment agent stirs 45min to waste water, and mixing speed 45r/min stands 15min later, to treated waste water
It is separated by solid-liquid separation, the additional amount of the dye wastewater treatment agent is the 0.5% of waste water from dyestuff weight to be processed.The nature sunlight
The intensity of illumination of irradiation or simulated solar irradiation irradiation is 50000LX or so.
Embodiment 8:
A kind of dye waste water treatment method, comprising the following steps:
The pH value of waste water from dyestuff is adjusted to 6, is placed under the irradiation of nature sunlight, the dye in the embodiment of the present invention 2 is added
Expect waste water treating agent, 50min stirred to waste water, mixing speed 50r/min stands 12min later, to treated waste water into
Row is separated by solid-liquid separation, and the additional amount of the dye wastewater treatment agent is the 0.2% of waste water from dyestuff weight to be processed.Natural sunlight irradiation
Intensity of illumination be 20000LX or so.
Embodiment 9:
A kind of dye waste water treatment method, comprising the following steps:
The pH value of waste water from dyestuff is adjusted to 7, is placed under simulated solar irradiation irradiation, the dye in the embodiment of the present invention 3 is added
Expect waste water treating agent, 40min stirred to waste water, mixing speed 30r/min stands 15min later, to treated waste water into
Row is separated by solid-liquid separation, and the additional amount of the dye wastewater treatment agent is the 0.7% of waste water from dyestuff weight to be processed.The simulated solar illumination
The intensity of illumination penetrated is 15000LX or so.
Embodiment 10:
A kind of dye waste water treatment method, comprising the following steps:
The pH value of waste water from dyestuff is adjusted to 5.5, is placed under simulated solar irradiation irradiation, dye wastewater treatment agent is added, it is right
Waste water stirs 35min, and mixing speed 40r/min stands 10min later, and to treated, waste water is separated by solid-liquid separation, the dye
The additional amount for expecting waste water treating agent is the 0.3% of waste water from dyestuff weight to be processed.The simulated solar irradiation irradiation intensity of illumination be
40000LX or so.
Comparative example 1:
A kind of dye waste water treatment method, dye wastewater treatment agent used are made of raw material from the following weight: PDMDAAC
72 parts of modification infusorial earth；6 parts of aluminium polychloride.Preparation method is stirred the following steps are included: weighing each raw material by recipe ratio and being placed in
It mixes in tank, 30min, mixing speed 800r/min is stirred at 55 DEG C.
Other steps of the dye waste water treatment method are the same as embodiment 7.
Comparative example 2:
A kind of dye waste water treatment method, dye wastewater treatment agent used are made of raw material from the following weight: cerium and gadolinium
Co-doped nano TiO20.3 part；6 parts of aluminium polychloride.Preparation method is the following steps are included: weigh each raw material simultaneously by recipe ratio
It is placed in agitator tank, 30min, mixing speed 800r/min is stirred at 55 DEG C.
Other steps of the dye waste water treatment method are the same as embodiment 7.
Comparative example 3:
A kind of dye waste water treatment method, dye wastewater treatment agent used, is made of raw material from the following weight: cerium and gadolinium
Co-doped nano TiO20.3 part；72 parts of PDMDAAC modification infusorial earth.Preparation method by recipe ratio the following steps are included: weighed
Each raw material is placed in agitator tank, and 30min, mixing speed 800r/min are stirred at 55 DEG C.
Other steps of the dye waste water treatment method are the same as embodiment 7.
Performance test:
Taking concentration is the methylene blue waste water of 30mg/L, Congo red waste water, Methyl Orange in Wastewater, uses embodiment respectively
Wastewater treatment method in 7-10 and comparative example 1-3 carries out wastewater treatment, and clear liquid is taken after separation of solid and liquid, measure absorption curve and its
Absorbance simultaneously calculates percent of decolourization η, and measures sample chemical oxygen demand according to national standard analysis method (GB 11914-89)
(COD) removal rate is to evaluate the performance that dye wastewater treatment agent of the present invention handles waste water from dyestuff.
The calculating formula of the percent of decolourization η and COD removal rate R of waste water from dyestuff is as follows:
η=1-At/A0；R=1-CODt/COD0。
In formula: A0And AtAbsorbance respectively after the initial and illumination t time of waste water from dyestuff, COD0And CODtRespectively
COD after the initial and illumination t time of waste water from dyestuff.Wherein decolorizing effect is as shown in table 1, and COD removal effect is as shown in table 2.
Table 1:
Table 2:
By table 1, table 2 it is found that the waste water treating agent in the present invention is excellent to the treatment effect of waste water from dyestuff, percent of decolourization, COD
Removal rate is high, good degrading effect.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. absorption/flocculation/photocatalysis composite dye waste water treating agent, which is characterized in that be made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.1-0.5 parts；
60-80 parts of PDMDAAC modification infusorial earth；
20-35 parts of inorganic polymer flocculant.
2. dye wastewater treatment agent according to claim 1, which is characterized in that be made of raw material from the following weight:
Cerium and gadolinium co-doped nano TiO20.3 part；
72 parts of PDMDAAC modification infusorial earth；
26 parts of inorganic polymer flocculant.
3. dye wastewater treatment agent according to claim 1, which is characterized in that the inorganic polymer flocculant is polymerization
One of aluminium chloride, polyaluminium sulfate, bodied ferric sulfate.
4. dye wastewater treatment agent according to claim 1, which is characterized in that the cerium and gadolinium co-doped nano TiO2's
Preparation method the following steps are included:
(1) a certain amount of ammonium hydroxide and hydrochloric acid are added into water, the buffer solution that pH value is 1.5-2.5 is made；Titanium tetrafluoride is molten
In above-mentioned buffer solution, 0.05molL is made-1Titanium tetrafluoride solution, adjust solution ph to 1.5-2；
(2) deionized water is added into titanium tetrafluoride solution, solution concentration is diluted to 0.003molL-1After be added it is a certain amount of
Gadolinium nitrate hexahydrate, cerous nitrate hexahydrate；It is subsequently placed in reactor, the isothermal reaction 15-17h at 165 DEG C；From
The heart is rinsed 3 times respectively with deionized water, dehydrated alcohol, gained powder is dried 20-24h in 100 DEG C of vacuum ovens, i.e.,
?.
5. dye wastewater treatment agent according to claim 1, which is characterized in that the cerium and gadolinium co-doped nano TiO2In,
Cerium, gadolinium, titanium atomic ratio be 0.5-1.5:0.3-0.8:100.
6. dye wastewater treatment agent according to claim 5, which is characterized in that the cerium and gadolinium co-doped nano TiO2In,
Cerium, gadolinium, titanium atomic ratio be 1:0.5:100.
7. dye wastewater treatment agent according to claim 1, which is characterized in that the system of the PDMDAAC modification infusorial earth
Preparation Method the following steps are included:
(1) 60-100 mesh is crossed after grinding diatomite, and the powder for being attached to diatomite surface is washed away with distilled water, is placed in 70-
Drying, takes out after 850 DEG C of calcination 1.5h of Muffle furnace, is cooled to room temperature in 80 DEG C of vacuum oven；
(2) it will be placed in through step (1) resulting diatomite in the sulfuric acid that mass concentration is 30-40% and carry out acidleach processing, filtered
Being washed repeatedly using water afterwards is neutrality to filtrate, then is placed in drying in 70-80 DEG C of vacuum oven；
(3) it will be mixed in an aqueous medium through step (2) resulting diatomite with PDMDAAC 1:0.02-0.045 in mass ratio,
Be stirred to react 2h at 65 DEG C, then filter, after being washed with water 3 times, be placed in 70-80 DEG C of vacuum oven drying to get.
8. dye wastewater treatment agent according to claim 1, which is characterized in that the preparation side of the dye wastewater treatment agent
Method is placed in agitator tank the following steps are included: weighing each raw material by recipe ratio, and 20~30min, stirring are stirred at 50-60 DEG C
Speed is 600-1200r/min.
9. a kind of dye waste water treatment method, which comprises the following steps:
The pH value of waste water from dyestuff is adjusted to 5.5-7, is placed under the irradiation of nature sunlight or under simulated solar irradiation irradiation, is added such as
Dye wastewater treatment agent of any of claims 1-8 stirs 40-50min, mixing speed 30-50r/ to waste water
Min stands 10-15min later, and to treated, waste water is separated by solid-liquid separation, and the additional amount of the dye wastewater treatment agent is
The 0.2-0.7% of waste water from dyestuff weight to be processed.
10. dye waste water treatment method according to claim 9, which is characterized in that the nature sunlight irradiation or mould
The intensity of illumination of quasi- sunlight irradiation is in 15000LX or more.
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| CN114604947A (en) * | 2022-03-21 | 2022-06-10 | 衡阳市建衡实业有限公司 | Titanium-containing composite ferric polysulfate flocculant and preparation method and application thereof |
| CN115477349A (en) * | 2022-10-17 | 2022-12-16 | 上海劲孚实业有限公司 | Wastewater treatment agent and preparation method thereof |
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Application publication date: 20190111 |