CN107983350A - A kind of preparation method of heterogeneous Fenton catalyst - Google Patents
A kind of preparation method of heterogeneous Fenton catalyst Download PDFInfo
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- CN107983350A CN107983350A CN201711071802.1A CN201711071802A CN107983350A CN 107983350 A CN107983350 A CN 107983350A CN 201711071802 A CN201711071802 A CN 201711071802A CN 107983350 A CN107983350 A CN 107983350A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000005909 Kieselgur Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 iron ion Chemical class 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 229910052598 goethite Inorganic materials 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
-
- 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
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation method of heterogeneous Fenton catalyst, comprises the following steps that：Step is as follows：Natural diatomaceous earth is cleaned, is precipitated, drying, roasts 2h at 350 DEG C, cools down；According to 1g:10ml, by diatomite and H2SO4Solution mixes, and stirs 1h, is washed till neutrality, dries；According to 1g:50ml, by diatomite and Fe (NO3)3Solution mixes, and 10min is stirred under the conditions of 60 DEG C, then instills the NaOH solution of same volume, continues to stir 2h, filters, rinses, drying, roasts 2h at 100 ~ 300 DEG C, heterogeneous Fenton catalyst is made.This method preparation process is easy to operate, and raw material is easy to get, and process is easy to control, catalyst reusable edible, non-secondary pollution, can realize effective degraded of COD and qualified discharge in beneficiation wastewater, have preferable application prospect.
Description
Technical field
The present invention relates to Industrial Wastewater Treatment and solid waste resource recovery to utilize field, particularly belongs to a kind of for degrading
The preparation of the heterogeneous Fenton catalyst of COD in beneficiation wastewater.
Technical background
Beneficiation wastewater is a kind of waste water common in mining production, with water is big, water quality is in sour or alkalescence, solid suspension
Thing is more, containing heavy metal ion and the features such as remaining beneficiation reagent, its COD generally can be higher, this is primarily due in ore dressing
The a large amount of all kinds of beneficiation reagents of Cheng Zhonghui additions, these beneficiation reagents can also remain in while valuable mineral recycling is helped
In final beneficiation wastewater so that the reductive organic matter too high levels that can be aoxidized in beneficiation wastewater, cause COD higher.
Fenton technologies are given up after the exploration and research of vast researcher for many years is passed through handling various difficult degradations
All achieved in terms of water compared with significant progress and development, according to the difference of chain carrier, gradually formed homogeneous Fenton
With two kinds of reaction systems of heterogeneous Fenton, such as lightwave CATV technology, Fenton technology, ultrasonic wave Fenton technologies etc. are all
Belong to the category of homogeneous Fenton.Heterogeneous Fenton catalyst be on the basis of traditional Fenton catalyst, by using
Iron content solid matter or carrier fix iron ion and H2O2The new Fenton oxidation System Catalyst of composition.It is heterogeneous
Fenton methods overcome traditional Fenton methods H2O2Utilization rate is low, Fe2+The shortcomings of easily bringing secondary pollution, becomes current waste water oxygen
Change a research hotspot in processing direction, one of important directions are the preparations of new heterogeneous Fenton catalyst, mesh
Be to obtain the catalyst that a kind of applicable pH range is wide, can recycle and recycle.
Fenton oxidation method has preferable treatment effect to the waste water containing organic pollution, more for containing in beneficiation wastewater
The organic beneficiation reagent of kind, the reality of COD high, it is a kind of compare to select a kind of more effectively Fenton catalyst to carry out degraded to it
Good thinking.Based on these features, Fenton oxidation method is improved, researches and develops more efficient heterogeneous Fenton oxidation side
Method, is a kind of effective thinking.
The nonmetallic mineral that diatomite is a kind of resource reserve very abundant, widely distributed and physicochemical properties protrude,
It has the characteristics that light, porous, specific surface area is big.Using diatomite it is easily modified, easily-activated, renewable the features such as carry out ring
The research of border protection, the particularly application in wastewater treatment etc., has very big Development volue.By tripolite loading iron oxygen
Compound is handled beneficiation wastewater for being catalyzed fenton-type reagent method, will increase substantially economy and environmental benefit, is mitigated
The environmental protection pressure of society.
The content of the invention
It is an object of the invention to provide a kind of preparation method of heterogeneous Fenton catalyst, which has preparation process
Simply, the catalyst ability of preparation is strong, H2O2Utilization rate is high, cost is low, improve Fenton methods obviously to choosing
The degradation efficiency of COD in ore deposit waste water, while there is stronger adaptation containing organic pollutant wastewater to the industrial and mining enterprises of complicated component
Property.
The preparation method step of the heterogeneous Fenton catalyst of the present invention is as follows：
1）Natural diatomaceous earth is cleaned, is precipitated, drying, roasts 2h at 350 DEG C, cools down；
2）According to 1g:10ml, by diatomite and H2SO4Solution mixes, and stirs 1h, is washed till neutrality, dries；
3）According to 1g:50ml, by diatomite and Fe (NO3)3Solution mixes, and 10min is stirred under the conditions of 60 DEG C, then instill identical
The NaOH solution of volume, continues to stir 2h, filters, rinse, drying, roasts 2h at 100 ~ 300 DEG C, obtained heterogeneous Fenton is urged
Agent.
The H2SO4The concentration of solution is 1mol/L.
Fe (the NO3)3The concentration of solution is 0.01 ~ 0.03mol/L.
The concentration of the NaOH solution is 0.03 ~ 0.15mol/L.
The diatomite is commercially available natural diatomaceous earth, which is SiO2, content 89.31%, particle diameter
For 2 ~ 220 μm, wherein D10=10.9 μm, D90=69.09 μm, mean particle size D50=32.77μm。
Catalyst SEM prepared by the method for the present invention show, and diatomite surface attachment one layer is loose, less uniformly and shaping
The unconspicuous material of state, EDS power spectrums show that this layer of newly-increased material is mainly goethite and amorphous Fe oxides mineral.Together
When diatomite also maintain certain duct and specific surface area, enable have with treating that degradation material more contacts site,
So as to reach more preferable catalytic action.BET test results show that the specific surface area of diatomite after supported ferriferous oxide is than natural silicon
Diatomaceous earth adds nearly 1.4 times, is conducive to it preferably and waste water, reaches catalytic degradation effect.
Embodiment
Following embodiments are intended only as illustrating the present invention, do not represent the limitation applied to the present invention.
Embodiment 1
Natural diatomaceous earth is cleaned, stood, is precipitated, is dried, is placed in Muffle furnace at 350 DEG C and roasts 2h, then cool down；
Diatomite powder is taken in dry beaker, adds the H that concentration is 1mol/L2SO4Solution, stirs 1h, cleans to neutrality, drying
It is spare.The purified pretreated diatom soil samples of 2.0g are weighed in 250ml beakers, it is 0.03mol/L to add 100ml concentration
Fe (NO3)3Solution, then in water bath with thermostatic control, keeps 60 DEG C of condition stirring 10min.Instilling 100ml concentration dropwise again is
The NaOH solution of 0.09mol/L, keeps 60 DEG C of waters bath with thermostatic control to continue to stir 2h, stands 24h, and filtering, rinse, drying, at 150 DEG C
2h is roasted, heterogeneous Fenton catalyst is made.
Embodiment 2
Natural diatomaceous earth is cleaned, stood, is precipitated, is dried, is placed in Muffle furnace at 350 DEG C and roasts 2h, then cool down；
Diatomite powder is taken in dry beaker, adds the H that concentration is 1mol/L2SO4Solution, stirs 1h, cleans to neutrality, drying
It is spare.The purified pretreated diatom soil samples of 2.0g are weighed in 250ml beakers, it is 0.03mol/L to add 100ml concentration
Fe (NO3)3Solution, then in water bath with thermostatic control, keeps 60 DEG C of condition stirring 10min.Instilling 100ml concentration dropwise again is
The NaOH solution of 0.03mol/L, keeps 60 DEG C of waters bath with thermostatic control to continue to stir 2h, stands 24h, and filtering, rinse, drying, at 150 DEG C
2h is roasted, heterogeneous Fenton catalyst is made.
Embodiment 3
Natural diatomaceous earth is cleaned, stood, is precipitated, is dried, is placed in Muffle furnace at 350 DEG C and roasts 2h, then cool down；
Diatomite powder is taken in dry beaker, adds the H that concentration is 1mol/L2SO4Solution, stirs 1h, cleans to neutrality, drying
It is spare.The purified pretreated diatom soil samples of 2.0g are weighed in 250ml beakers, it is 0.03mol/L to add 100ml concentration
Fe (NO3)3Solution, then in water bath with thermostatic control, keeps 60 DEG C of condition stirring 10min.Instilling 100ml concentration dropwise again is
The NaOH solution of 0.09mol/L, keeps 60 DEG C of waters bath with thermostatic control to continue to stir 2h, stands 24h, and filtering, rinse, drying, at 250 DEG C
2h is roasted, heterogeneous Fenton catalyst is made.
Embodiment 4
Natural diatomaceous earth is cleaned, stood, is precipitated, is dried, is placed in Muffle furnace at 350 DEG C and roasts 2h, then cool down；
Diatomite powder is taken in dry beaker, adds the H that concentration is 1mol/L2SO4Solution, stirs 1h, cleans to neutrality, drying
It is spare.The purified pretreated diatom soil samples of 2.0g are weighed in 250ml beakers, it is 0.02mol/L to add 100ml concentration
Fe (NO3)3Solution, then in water bath with thermostatic control, keeps 60 DEG C of condition stirring 10min.Instilling 100ml concentration dropwise again is
The NaOH solution of 0.06mol/L, keeps 60 DEG C of waters bath with thermostatic control to continue to stir 2h, stands 24h, and filtering, rinse, drying, at 150 DEG C
2h is roasted, heterogeneous Fenton catalyst is made.
The beneficiation wastewater 100ml that COD is 188mg/L is taken, it is 5 to adjust raw water pH, adds above-described embodiment 1 ~ 4 of 1.5g/L
Catalyst and 11.79mmol/L H2O2, stirring reaction, is subsequently placed in ultrasonic cleaner, is reacted under 40kHz, 80W
60min, stands, is layered, filtering, the COD changes before and after wastewater treatment is measured, after measured, in the beneficiation wastewater of embodiment 1 ~ 4
The removal rate of COD is respectively 85.61%, 63.24%, 68.58% and 74.22%.
Claims (4)
- A kind of 1. preparation method of heterogeneous Fenton catalyst, it is characterized in that step is as follows：1）Natural diatomaceous earth is cleaned, is precipitated, drying, roasts 2h at 350 DEG C, cools down；2）According to 1g:10ml, by diatomite and H2SO4Solution mixes, and stirs 1h, is washed till neutrality, dries；3）According to 1g:50ml, by diatomite and Fe (NO3)3Solution mixes, and 10min is stirred under the conditions of 60 DEG C, then instill identical The NaOH solution of volume, continues to stir 2h, filters, rinse, drying, roasts 2h at 100 ~ 300 DEG C, obtained heterogeneous Fenton is urged Agent.
- 2. the preparation method of heterogeneous Fenton catalyst according to claim 1, it is characterized in that the H2SO4Solution Concentration is 1mol/L.
- 3. the preparation method of heterogeneous Fenton catalyst according to claim 1 the, it is characterized in that Fe (NO3)3Solution Concentration be 0.01 ~ 0.03mol/L.
- 4. the preparation method of heterogeneous Fenton catalyst according to claim 1, it is characterized in that the NaOH solution Concentration is 0.03 ~ 0.15mol/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711071802.1A CN107983350A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of heterogeneous Fenton catalyst |
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| CN201711071802.1A CN107983350A (en) | 2017-11-03 | 2017-11-03 | A kind of preparation method of heterogeneous Fenton catalyst |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318132A (en) * | 2007-06-08 | 2008-12-10 | 中山大学 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
| CN103285887A (en) * | 2013-06-09 | 2013-09-11 | 吉林市英达水务科技有限责任公司 | Kieselguhr loading solid superacid type Fenton catalyst preparation method |
-
2017
- 2017-11-03 CN CN201711071802.1A patent/CN107983350A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318132A (en) * | 2007-06-08 | 2008-12-10 | 中山大学 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
| CN103285887A (en) * | 2013-06-09 | 2013-09-11 | 吉林市英达水务科技有限责任公司 | Kieselguhr loading solid superacid type Fenton catalyst preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 梁欢: "硅藻土基非均相Fenton催化材料的制备及其降解染料废水的研究", 《中国博士论文全文库工程科技I辑》 * |
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Application publication date: 20180504 |