CN108940309A - A kind of preparation method of the catalysis reduction bed of rapid sewage treating - Google Patents
A kind of preparation method of the catalysis reduction bed of rapid sewage treating Download PDFInfo
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- CN108940309A CN108940309A CN201810796455.7A CN201810796455A CN108940309A CN 108940309 A CN108940309 A CN 108940309A CN 201810796455 A CN201810796455 A CN 201810796455A CN 108940309 A CN108940309 A CN 108940309A
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- bamboo charcoal
- charcoal particle
- negative pressure
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- 238000002360 preparation method Methods 0.000 title claims abstract description 60
- 239000010865 sewage Substances 0.000 title claims abstract description 34
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 33
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims abstract description 91
- 235000017491 Bambusa tulda Nutrition 0.000 claims abstract description 91
- 241001330002 Bambuseae Species 0.000 claims abstract description 91
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims abstract description 91
- 239000011425 bamboo Substances 0.000 claims abstract description 91
- 239000003610 charcoal Substances 0.000 claims abstract description 90
- 239000002245 particle Substances 0.000 claims abstract description 86
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000243 solution Substances 0.000 claims abstract description 50
- 239000011259 mixed solution Substances 0.000 claims abstract description 45
- 238000002386 leaching Methods 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000007603 infrared drying Methods 0.000 claims abstract description 26
- 238000005470 impregnation Methods 0.000 claims abstract description 25
- 230000004913 activation Effects 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 56
- 238000006243 chemical reaction Methods 0.000 claims description 51
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000002585 base Substances 0.000 claims description 23
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 16
- 229910052697 platinum Inorganic materials 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 16
- 229910052719 titanium Inorganic materials 0.000 claims description 16
- 239000012279 sodium borohydride Substances 0.000 claims description 13
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 13
- 230000004224 protection Effects 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003513 alkali Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract description 2
- 241000894006 Bacteria Species 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000010841 municipal wastewater Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001546 nitrifying effect Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000452 restraining effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8946—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with alkali or alkaline earth metals
-
- B01J35/50—
-
- 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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
Abstract
The present invention provides a kind of preparation method of the catalysis reduction bed of rapid sewage treating, and this method includes Fe-base Solution preparation, mixed solution I preparation, mixed solution I I preparation, high-temperature activation bamboo charcoal particle, negative pressure leaching infrared drying, negative pressure impregnation, negative pressure leaching, infrared drying and high temperature sintering.The present invention provides one kind using bamboo charcoal particle as carrier, loading to it has the more metal mixtures of very high activity, sintering means are controlled by temperature, metal mixture is securely attached on bamboo charcoal particle, the catalytic reducer of high activity is generated under hydrolysis, ammonia nitrogen and nitrogen are catalysed and reduced into the nitrate nitrogen in polluted-water, achieve the purpose that denitrogenation.
Description
[technical field]
The present invention relates to technical field of sewage, and in particular to a kind of preparation of the catalysis reduction bed of rapid sewage treating
Method.
[background technique]
Sewage treatment both at home and abroad at present is for the denitrifying bacterium that the mainstream processing method of nitrate nitrogen is using culture domestication
Group, reduction decomposition nitrate nitrogen generates gaseous state nitride and nitrogen under anaerobic state, and is limited by biological treatment, instead
Time required for time required for nitrifying process and subsequent digestion process be extremely difficult to unification, be denitrification efficiency significantly
Reducing this is one of restraining factors, another factor restricted is the dense of required organic carbon source in denitrifying bacterium growth cycle
Degree whether enough denitrifying bacterium demands, while outside air temperature and sewage organic pollutant concentration are mostly to influence denitrifying bacterium reduction nitre
The factor of sour nitrogen efficiency.
[summary of the invention]
In view of the foregoing, it is necessary to which a kind of preparation method of the catalysis reduction bed of rapid sewage treating is provided.
In order to achieve the above objectives, the technical scheme adopted by the invention is that: a kind of catalysis of rapid sewage treating restores bed
Preparation method, the preparation method the following steps are included:
S1, Fe-base Solution preparation, water and ethyl alcohol are poured into reaction kettle, are opened nitrogen valve and are started blender, stir 30min
Iron chloride is put into reaction kettle afterwards, continues to stir 120min, obtains Fe-base Solution;
Butyl titanate is instilled in dehydrated alcohol under stirring and obtains titanium colloidal sol drop, by titanium by S2, mixed solution I preparation
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Further, in step sl, the volumetric ratio of water and ethyl alcohol are as follows: 1:0.5.
Further, in step sl, iron chloride is 0.25-0.65 moles.
Further, in step s 2, butyl titanate is 0.25-0.65 moles.
Further, in step s3, chloroplatinic acid is 0.001-0.005 moles.
Further, in step s 6, sodium borohydride is 0.45 mole.
Further, in step s 4, the bamboo charcoal particle partial size is 5-10mm, in 650 DEG C of nitrogen after alkali steeps pickling
It is activated under gas shielded.
Further, in step s 4, the volumetric ratio of bamboo charcoal particle and mixed solution I I are 1:1.
Further, in step s 6, the volumetric ratio of bamboo charcoal particle and sodium borohydride are as follows: 1:1.2.
Compared with the prior art, the invention has the following advantages:
The present invention provides one kind using bamboo charcoal particle as carrier, and loading to it has the more metal mixtures of very high activity, leads to
Excess temperature controls sintering means, and metal mixture is securely attached on bamboo charcoal particle, and high activity is generated under hydrolysis
Catalytic reducer is catalysed and reduced into ammonia nitrogen and nitrogen to the nitrate nitrogen in polluted-water, achievees the purpose that denitrogenation.
[Detailed description of the invention]
Fig. 1 is a flow chart of the preparation method of the catalysis reduction bed of rapid sewage treating of the invention.
[specific embodiment]
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical;Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention;Description and claims of this specification and above-mentioned attached drawing are said
Term " includes " in bright and " having " and their any deformation, it is intended that cover and non-exclusive include.
Referenced herein " embodiment " is it is meant that a particular feature, structure, or characteristic described can wrap in conjunction with the embodiments
Containing at least one embodiment of the present invention.Each position in the description occur the phrase might not each mean it is identical
Embodiment, nor the independent or alternative embodiment with other embodiments mutual exclusion.Those skilled in the art explicitly and
Implicitly understand, embodiment described herein can be combined with other embodiments.
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described.
Embodiment 1
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in first embodiment of the invention
Preparation Method, the preparation method the following steps are included:
S1, Fe-base Solution preparation, water and ethyl alcohol are poured into reaction kettle, are opened nitrogen valve and are started blender, stir 30min
Iron chloride is put into reaction kettle afterwards, continues to stir 120min, obtains Fe-base Solution;
S2, mixed solution I preparation instill in dehydrated alcohol under stirring in butyl titanate and obtain titanium colloidal sol drop, by titanium
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Embodiment 2
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in second embodiment of the present invention
Preparation Method, the preparation method the following steps are included:
Water and ethyl alcohol that volumetric ratio is 1:0.5 are poured into reaction kettle, open nitrogen valve starting by S1, Fe-base Solution preparation
Blender puts into 0.25-0.65 moles of iron chloride in reaction kettle after stirring 30min, continues to stir 120min, obtain iron-based molten
Liquid;
Butyl titanate is instilled in dehydrated alcohol under stirring and obtains titanium colloidal sol drop, by titanium by S2, mixed solution I preparation
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Embodiment 3
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in third embodiment of the present invention
Preparation Method, the preparation method the following steps are included:
Water and ethyl alcohol that volumetric ratio is 1:0.5 are poured into reaction kettle, open nitrogen valve starting by S1, Fe-base Solution preparation
Blender puts into iron chloride in reaction kettle after stirring 30min, continues to stir 120min, obtains Fe-base Solution;
S2, mixed solution I preparation, 0.25-0.65 moles of butyl titanate is instilled in dehydrated alcohol under stirring
Titanium colloidal sol drop is obtained, titanium colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, reaction kettle works under nitrogen protection stirring,
Obtain mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Embodiment 4
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in the 4th embodiment of the invention
Preparation Method, the preparation method the following steps are included:
Water and ethyl alcohol that volumetric ratio is 1:0.5 are poured into reaction kettle, open nitrogen valve starting by S1, Fe-base Solution preparation
Blender puts into iron chloride in reaction kettle after stirring 30min, continues to stir 120min, obtains Fe-base Solution;
Butyl titanate is instilled in dehydrated alcohol under stirring and obtains titanium colloidal sol drop, by titanium by S2, mixed solution I preparation
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in 0.45 mole of sodium borohydride solution
120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Embodiment 5
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in the 5th embodiment of the invention
Preparation Method, the preparation method the following steps are included:
S1, Fe-base Solution preparation, water and ethyl alcohol are poured into reaction kettle, are opened nitrogen valve and are started blender, stir 30min
Iron chloride is put into reaction kettle afterwards, continues to stir 120min, obtains Fe-base Solution;
S2, mixed solution I preparation instill in dehydrated alcohol under stirring in butyl titanate and obtain titanium colloidal sol drop, by titanium
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;Preferably, the bamboo charcoal
Grain diameter is 5-10mm, is activated under 650 DEG C of nitrogen protections after alkali steeps pickling;The appearance of bamboo charcoal particle and mixed solution I I
Product is than being 1:1;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
Embodiment 6
Referring to Fig. 1, providing a kind of system of the catalysis reduction bed of rapid sewage treating in sixth embodiment of the invention
Preparation Method, the preparation method the following steps are included:
S1, Fe-base Solution preparation, water and ethyl alcohol are poured into reaction kettle, are opened nitrogen valve and are started blender, stir 30min
Iron chloride is put into reaction kettle afterwards, continues to stir 120min, obtains Fe-base Solution;
S2, mixed solution I preparation instill in dehydrated alcohol under stirring in butyl titanate and obtain titanium colloidal sol drop, by titanium
Colloidal sol is added dropwise in the Fe-base Solution in reaction kettle, and reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, will prepare
Platinum solution pour into reaction kettle continue stir 30min, obtain mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into after being sufficiently mixed by the bamboo charcoal particle of pretreatment high-temperature activation
In reaction kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, starts vacuum pump
It stands and takes out negative pressure 120min, be mixing liquid well into the gap of bamboo charcoal particle, be aged 6-8h;Preferably, the bamboo charcoal
Grain diameter is 5-10mm, is activated under 650 DEG C of nitrogen protections after alkali steeps pickling;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into red
In outer baking oven 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;Preferably,
The volumetric ratio of bamboo charcoal particle and sodium borohydride are as follows: 1:1.2;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of
Toast 120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, obtained after natural cooling by S9, high temperature sintering
Required catalysis restores bed.
The catalysis reduction bed for the rapid sewage treating being prepared according to the preparation method of Examples 1 to 6 is in sewage
Nitrate nitrogen carries out direct-reduction decomposition, is that biological denitrification method effect increases 3-6 times, energy consumption reduces by 50% or more.
Wastewater treatment efficiency in order to better illustrate the present invention, is tested as follows:
1. equipment: special organic glass column type reactor, total high 1500mm, diameter of phi 200mm load carrier stack layer
High 1000mm.
Sewage pump: peristaltic pump, flow 0-50L/h.
Flowmeter: glass rotameter
2. analysis instrument:
Spectrophotometer
Clear up instrument
Pressure cooker
Vessel
3. step:
3.1 are stored in plastic barrel from the sanitary sewage that municipal wastewater drawing comes, and starting sewage pump flowmeter adjusts flow, from
Reaction column bottom enters catalytic oxidation bed, loads carrier height 1000mm, reduction column effective height 1200mm;Participate in reaction
Reactor is discharged from reaction column column top liquid stream in water body afterwards.
3.2 press different hydraulic detention times, and to treated, water sampling is analyzed:
Total residence time 30 minutes (mg/l)
Pollutant | TN | NH4-N | Phenomenon |
Raw water | 128 | 23.65 | It is yellowish, have peculiar smell, muddiness |
Oxidation bed water outlet | 14.72 | 47.86↑ | Transparent free from extraneous odour, ammonia nitrogen value increase |
Removal rate % | 88.50 | 2 weeks average of continuous operation |
Total residence time 60 minutes
Pollutant | TN | NH4-N | Phenomenon |
Raw water | 147 | 26.14 | It is yellowish, have peculiar smell, muddiness |
Oxidation water outlet | 9.43 | 52.48↑ | Transparent free from extraneous odour, ammonia nitrogen value increase |
Removal rate | 93.58 | 4 weeks average of continuous operation |
Total residence time 120 minutes
Pollutant | TN | NH4-N | Phenomenon |
Raw water | 135 | 31.45 | It is yellowish, have peculiar smell, muddiness |
Oxidation water outlet | 5.14 | 63.15↑ | Transparent free from extraneous odour, ammonia nitrogen value increase |
Removal rate | 96.19 | 4 weeks average of continuous operation |
It follows that a kind of rapid sewage treating provided by the invention catalysis reduction bed preparation method at least have as
It is lower the utility model has the advantages that
1, carrier of the present invention is bamboo charcoal particle, and bamboo resource distribution is wide to belong to reproducible utilization resource;
2, bamboo charcoal hole is evenly distributed then includes Determination of multiple metal elements abundant, the alloying metal grafting for being easy to load;
3, bamboo charcoal has specific surface area huge as carrier, and the contact after supported catalyst alloy material with water body increases, and subtracts
The residence time of few sewage and carrier contact, reactor volume is maximumlly reduced, treatment effeciency is improved;
4, the present invention nitrate nitrogen total to sewage carries out direct-reduction decomposition, is that biological denitrification method effect increases 3-6
Times, energy consumption reduces by 50% or more;
5, the present invention reaches 80% or more to the removal rate of the nitrate nitrogen in polluted-water;
6, the process that nitrate nitrogen restores in water body is NO3-N+H+--NH4-N+N2.
Obviously, embodiments described above is only a part of the embodiment of the present invention, instead of all the embodiments, attached
Presently preferred embodiments of the present invention is given in figure, but is not intended to limit the scope of the patents of the invention.The present invention can be with many differences
Form realize, on the contrary, purpose of providing these embodiments is keeps the understanding to the disclosure more thorough
Comprehensively.Although the present invention is described in detail referring to the foregoing embodiments, for coming for those skilled in the art,
Can still modify to technical solution documented by aforementioned each specific embodiment, or to part of technical characteristic into
Row equivalence replacement.All equivalent structures done using description of the invention and accompanying drawing content, are directly or indirectly used in other
Relevant technical field, similarly within the invention patent protection scope.
Claims (10)
1. a kind of preparation method of the catalysis reduction bed of rapid sewage treating, it is characterised in that: the preparation method includes following
Step:
S1, Fe-base Solution preparation, water and ethyl alcohol are poured into reaction kettle, are opened nitrogen valve and are started blender, will after stirring 30min
Iron chloride is put into reaction kettle, is continued to stir 120min, is obtained Fe-base Solution;
Butyl titanate is instilled in dehydrated alcohol under stirring and obtains titanium colloidal sol drop, by titanium colloidal sol by S2, mixed solution I preparation
It is added dropwise in the Fe-base Solution in reaction kettle, reaction kettle works under nitrogen protection stirring, obtains mixed solution I;
S3, mixed solution I I preparation, chloroplatinic acid is added in deionized water, is stirred 120min, is obtained platinum solution, the platinum that will be prepared
Solution, which pours into reaction kettle, to be continued to stir 30min, obtains mixed solution I I;
S4, high-temperature activation bamboo charcoal particle will be poured slowly into reaction by the bamboo charcoal particle of pretreatment high-temperature activation after being sufficiently mixed
In kettle, stirring 60min contacts bamboo charcoal particle and mixed solution I I uniformly, closes nitrogen valve and stirring, and starting vacuum pump is stood
Negative pressure 120min is taken out, is mixing liquid well into the gap of bamboo charcoal particle, is aged 6-8h;
S5, negative pressure leaching infrared drying, the bamboo charcoal particle after taking out ageing are put into negative pressure leaching in nutsch filter, place into infrared baking
In case 120 DEG C at a temperature of dry;
S6, negative pressure impregnation, by the bamboo charcoal particle negative pressure impregnation after drying in sodium borohydride solution 120min;
Bamboo charcoal particle taking-up after negative pressure impregnation is placed again into vacuumfilter by S7, negative pressure leaching;
Bamboo charcoal particle after negative pressure leaching is placed again into infrared baking oven by S8, infrared drying, 120 DEG C at a temperature of toast
120min;
Bamboo charcoal particle after infrared drying is put into temperature control in high temperature furnace and is sintered, needed for obtaining after natural cooling by S9, high temperature sintering
The catalysis reduction bed wanted.
2. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as described in claim 1, it is characterised in that: in step
In rapid S1, the volumetric ratio of water and ethyl alcohol are as follows: 1:0.5.
3. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 2, it is characterised in that: in step
In rapid S1, iron chloride is 0.25-0.65 moles.
4. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 2, it is characterised in that: in step
In rapid S2, butyl titanate is 0.25-0.65 moles.
5. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 2, it is characterised in that: in step
In rapid S3, chloroplatinic acid is 0.001-0.005 moles.
6. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 2, it is characterised in that: in step
In rapid S6, sodium borohydride is 0.45 mole.
7. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as described in claim 1, it is characterised in that: in step
In rapid S4, the bamboo charcoal particle partial size is 5-10mm, is activated under 650 DEG C of nitrogen protections after alkali steeps pickling.
8. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 7, it is characterised in that: in step
In rapid S4, the volumetric ratio of bamboo charcoal particle and mixed solution I I are 1:1.
9. a kind of preparation method of the catalysis reduction bed of rapid sewage treating as claimed in claim 7, it is characterised in that: in step
In rapid S6, the volumetric ratio of bamboo charcoal particle and sodium borohydride are as follows: 1:1.2.
10. a kind of catalysis of rapid sewage treating restores bed, it is characterised in that: using any one of claim 1~9 preparation side
Method is prepared.
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CN110316895A (en) * | 2019-08-06 | 2019-10-11 | 东北师范大学 | A kind of processing method of the industrial wastewater containing high concentration nitrate |
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