CN107159113B - It is a kind of for adsorbing the load TiO of xanthate2Active carbon and preparation method thereof and adsorption method - Google Patents
It is a kind of for adsorbing the load TiO of xanthate2Active carbon and preparation method thereof and adsorption method Download PDFInfo
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- CN107159113B CN107159113B CN201710392513.5A CN201710392513A CN107159113B CN 107159113 B CN107159113 B CN 107159113B CN 201710392513 A CN201710392513 A CN 201710392513A CN 107159113 B CN107159113 B CN 107159113B
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- xanthate
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 126
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims abstract description 101
- 239000012991 xanthate Substances 0.000 claims abstract description 101
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000002351 wastewater Substances 0.000 claims abstract description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 13
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000013049 sediment Substances 0.000 claims description 16
- 238000010521 absorption reaction Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 230000008595 infiltration Effects 0.000 claims 1
- 238000001764 infiltration Methods 0.000 claims 1
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 14
- 238000001914 filtration Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 10
- -1 alkyl dithiocarbonate Chemical compound 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000005188 flotation Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- TUZCOAQWCRRVIP-UHFFFAOYSA-N butoxymethanedithioic acid Chemical group CCCCOC(S)=S TUZCOAQWCRRVIP-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 208000004756 Respiratory Insufficiency Diseases 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 201000004193 respiratory failure Diseases 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of for adsorbing the load TiO of xanthate2Active carbon, including following material composition: butyl titanate, dehydrated alcohol and active carbon.Preparation method includes the following steps, first mixes butyl titanate with dehydrated alcohol, stirs to obtain yellow transparent solution, and be added dropwise to HNO3In solution, continues to stir, obtain TiO2Colloidal sol；TiO is added in active carbon2In colloidal sol, stirring is layered after standing, taking precipitate and successively drying, calcining to get.Also disclose the load TiO for adsorbing xanthate2The adsorption method of active carbon: it will be used to adsorb the load TiO of xanthate2Active carbon is placed in the waste water containing xanthate, standing adsorption 10-90min.The load TiO for being used to adsorb xanthate of the invention2Active carbon is not soluble in water, and property is stablized, nuisanceless to environment, under alkaline condition, significantly improves active carbon to the adsorption rate of xanthate, and can extend load TiO2Active carbon recycles the service life.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of for adsorbing the load TiO of xanthate2Active carbon and
Preparation method and adsorption method.
Background technique
With China's expanding economy, free-milling ore is fewer and fewer, and the exploitation of poor thin matrix is more and more.Refractory ore
Usually require the more beneficiation reagents of consumption.Beneficiation wastewater is directly to environmental emission meeting polluted river, the meeting again of waste water recycling water utilization
Adverse effect is caused to production.
The entitled alkyl dithiocarbonate of xanthate chemistry, commonly known as xanthates, by alkyl (R), the solid (OCSS of parent-)
And alkali metal Me (Na+、K+) composition, it is divided into ethyl xanthate, butyl xanthate, amyl group xanthate etc..Xanthate is soluble easily in water, and in water
Hydrolysis easily occurs, decomposes, has the advantages that easily manufacture, price is low etc., is that current flotation metal sulfide ore is most widely used, most effective
Collecting agent.But xanthate Central nervous is inhibited, when accumulation arrives a certain amount of in vivo, animal can be made dead
In respiratory failure, when having 2#In the presence of oil, due to the effect of synergistic effect, the toxicity of xanthate is obviously increased.
Currently, active carbon adsorption is processing flotation waste water a kind of commonly method, but since non-ferrous metal ore is more
It carries out under alkaline condition, due to OH under alkaline condition-The competitive Adsorption of ion acts on, and active carbon can show the adsorbance of xanthate
Write decline.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide a kind of for adsorbing the load of xanthate
TiO2Active carbon and preparation method thereof and adsorption method.Load TiO2The preparation method of active carbon is simple, and it is floating to be used for absorption
When selecting the xanthate in waste water, it is remarkably improved the adsorption rate to xanthate under alkaline condition.
In order to achieve the above object, the present invention is achieved by the following scheme.
(1) a kind of for adsorbing the load TiO of xanthate2Active carbon, which is characterized in that including following material composition: metatitanic acid
Butyl ester, dehydrated alcohol and active carbon.
Preferably, the ratio of the tetraethyl titanate, dehydrated alcohol and the active carbon is (2-4) mL: (5-10) mL: 1g.
Preferably, described for adsorbing the load TiO of xanthate2Active carbon further includes HNO3Solution.
It is further preferred that the HNO3The substance withdrawl syndrome of solution is 1mol/L, and the HNO3Solution and the work
Property charcoal ratio be 10mL: 1g.
(2) a kind of for adsorbing the load TiO of xanthate2The preparation method of active carbon, which is characterized in that including following step
It is rapid:
Step 1, butyl titanate is mixed with dehydrated alcohol, 15-30 min is stirred under the speed of 400-600r/min, is obtained
Yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to HNO3In solution, after being added dropwise to complete, continues to stir 2-3h, be used in combination
NaOH solution adjusts pH to 1-2, and 20-30min is sufficiently stirred, obtains TiO2Colloidal sol；
Step 3, the TiO is added in active carbon2It in colloidal sol, stirs, is layered after standing, sediment is taken out, by sediment
It is dried under the conditions of 80-100 DEG C, and calcines 1-3h under the conditions of 400-500 DEG C to get load TiO2Active carbon.
Preferably, in step 2, the HNO3Solution is in stirring, and mixing speed is 800-1000 r/min, institute
Stating the time being added dropwise to complete is 1-2h.
Preferably, in step 2, the speed being sufficiently stirred is 400-600r/min.
Preferably, described that the TiO is added in active carbon in step 32Before in colloidal sol, the active carbon is added first
Enter and infiltrates 1-2h in water.
Preferably, in step 3, the time of the stirring is 18-24h, and the speed of the stirring is 400-600 r/min.
Preferably, in step 3, the calcining is in N2It is carried out under protection environment.
(3) a kind of for adsorbing the load TiO of xanthate2The adsorption method of active carbon, which is characterized in that according to following step
It is rapid to carry out: by the load TiO for being used to adsorb xanthate2Active carbon is placed in the waste water containing xanthate, standing adsorption.
Preferably, the waste water containing xanthate is alkalinity.
Preferably, the time of the standing adsorption is 10-90min.
Preferably, described for adsorbing the load TiO of xanthate2The ratio of adsorption of active carbon and the waste water containing xanthate
It is 0.03g: (30-50) mL.
It is further preferred that the concentration of the waste water containing xanthate is 8-12mg/L.
Compared with prior art, the invention has the benefit that
Provided by the present invention for adsorbing the load TiO of xanthate2Active carbon is not soluble in water, and property is stablized, to environment without public affairs
Evil.When being applied to waste water of the purification containing xanthate, due to loading TiO2Improve specific surface area and the micropore hole of active carbon
Gap rate does not use ultraviolet irradiation condition, load TiO of the invention under alkaline condition2Absorption of the active carbon to ethyl xanthate
Rate improves 20-23%；Under alkaline condition, under conditions of using ultraviolet irradiation, load TiO of the invention2Active carbon is to second
The adsorption rate of base xanthate improves 29%.In addition, load TiO2It can be utilized, and recycled with activation cycle after active carbon use
Using to TiO2Catalytic oxidation performance and active carbon activity influence it is smaller；Due to TiO2It can will be adsorbed under ultraviolet irradiation
Xanthate rapid oxidation, make activated carbon surface keep activity, extend active carbon recycles the service life.
Detailed description of the invention
The present invention is described in further details in the following with reference to the drawings and specific embodiments.
Fig. 1 is of the invention for adsorbing the load TiO of xanthate2Active carbon and active carbon carry out the waste water containing xanthate
Absorption result figure after absorption；Wherein, a curve is of the invention for adsorbing the load TiO of xanthate2Active carbon is to containing xanthate
Waste water adsorbed after absorption result, b curve be active carbon the waste water containing xanthate is adsorbed after absorption result,
C point is of the invention for adsorbing the load TiO of xanthate2Active carbon adsorbs the waste water containing xanthate under ultraviolet irradiation
Absorption result after 90min.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
It will be appreciated that the following example is merely to illustrate the present invention, and it is not construed as limiting the scope of the invention.
Embodiment 1
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 80mL butyl titanate and 100mL dehydrated alcohol to mix, stirs 30min under the speed of 500r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 1h is added dropwise, drips
Cheng Hou continues to stir 3h, and adjusts pH to 1 with NaOH solution, and 30min is sufficiently stirred under the speed of 500r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 1h, be added into the TiO2In colloidal sol, stirring
18h is layered after standing, is taken out sediment, sediment is dried under the conditions of 80 DEG C, and calcine 1h under the conditions of 450 DEG C, i.e.,
TiO must be loaded2Active carbon.
Embodiment 2
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 80mL butyl titanate and 150mL dehydrated alcohol to mix, stirs 15min under the speed of 400r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 1h is added dropwise, drips
Cheng Hou continues to stir 2h, and adjusts pH to 1 with NaOH solution, and 30min is sufficiently stirred under the speed of 500r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 1h, be added into the TiO2In colloidal sol, stirring
20h is layered after standing, is taken out sediment, sediment is dried under the conditions of 80 DEG C, and calcine 0.5h under the conditions of 500 DEG C,
Up to load TiO2Active carbon.
Embodiment 3
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 80mL butyl titanate and 200mL dehydrated alcohol to mix, stirs 30min under the speed of 600r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 2h is added dropwise, drips
Cheng Hou continues to stir 3h, and adjusts pH to 1.5 with NaOH solution, and 30min is sufficiently stirred under the speed of 400r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 2h, be added into the TiO2In colloidal sol, stirring
For 24 hours, it is layered after standing, takes out sediment, sediment is dried under the conditions of 80 DEG C, and calcine 1h under the conditions of 550 DEG C, i.e.,
TiO must be loaded2Active carbon.
Embodiment 4
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 40mL butyl titanate and 100mL dehydrated alcohol to mix, stirs 30min under the speed of 500r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 1h is added dropwise, drips
Cheng Hou continues to stir 2h, and adjusts pH to 1 with NaOH solution, and 30min is sufficiently stirred under the speed of 500r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 1.5h, be added into the TiO2In colloidal sol, stir
18h is mixed, is layered after standing, sediment is taken out, sediment is dried under the conditions of 80 DEG C, and calcine 1h under the conditions of 450 DEG C, i.e.,
TiO must be loaded2Active carbon.
Embodiment 5
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 60mL butyl titanate and 100mL dehydrated alcohol to mix, stirs 30min under the speed of 500r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 1h is added dropwise, drips
Cheng Hou continues to stir 2h, and adjusts pH to 1 with NaOH solution, and 30min is sufficiently stirred under the speed of 500r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 1.5h, be added into the TiO2In colloidal sol, stir
18h is mixed, is layered after standing, sediment is taken out, sediment is dried under the conditions of 80 DEG C, and calcine 1h under the conditions of 450 DEG C, i.e.,
TiO must be loaded2Active carbon.
Embodiment 6
For adsorbing the load TiO of xanthate2Active carbon is prepared according to the following steps:
Step 1, it takes 60mL butyl titanate and 200mL dehydrated alcohol to mix, stirs 30min under the speed of 400r/min,
Obtain yellow transparent solution；
Step 2, the yellow transparent solution is added dropwise to the HNO of 200mL 1mol/L3In solution, 2h is added dropwise, drips
Cheng Hou continues to stir 2h, and adjusts pH to 1 with NaOH solution, and 30min is sufficiently stirred under the speed of 500r/min, obtains
TiO2Colloidal sol；
Step 3, it takes 20g active carbon to be added in 200mL distilled water and infiltrates 1.5h, be added into the TiO2In colloidal sol, stir
18h is mixed, is layered after standing, sediment is taken out, sediment is dried under the conditions of 80 DEG C, and calcine 1h under the conditions of 450 DEG C, i.e.,
TiO must be loaded2Active carbon.
Active carbon in above-described embodiment 1-6 is using cocoanut active charcoal, the load for being used to adsorb xanthate of the invention
TiO2Active carbon in the raw material of active carbon is also possible to other kinds of active carbon.
Embodiment 7
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；Prepare 50mL 10mg/L ethyl
Xanthate solution is spare as the waste water containing xanthate；By weighed load TiO2It is molten that prepared ethyl xanthate is added in active carbon
In liquid, its pH value is adjusted to 11 with 1mol/L NaOH solution, standing adsorption 70min；Suspension is obtained after standing, and to suspension
Filtering, obtains filtrate and active carbon after filtering, filtrate is the waste water after handling, the active carbon reproducible utilization being obtained by filtration.
Embodiment 8
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；Prepare 30mL 12mg/L ethyl
Xanthate solution is spare as the waste water containing xanthate；By weighed load TiO2It is molten that prepared ethyl xanthate is added in active carbon
In liquid, its pH value is adjusted to 11 with 1mol/L NaOH solution, standing adsorption 30min；Suspension is obtained after standing, and to suspension
Filtering, obtains filtrate and active carbon after filtering, filtrate is the waste water after handling, the active carbon reproducible utilization being obtained by filtration.
Embodiment 9
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；It is yellow to prepare 30mL 8mg/L ethyl
Drug solns are spare as the waste water containing xanthate；By weighed load TiO2Prepared ethyl xanthate solution is added in active carbon
In, its pH value is adjusted to 11 with 1mol/L NaOH solution, standing adsorption 10min；Suspension is obtained after standing, and to suspension mistake
Filter, obtains filtrate and active carbon after filtering, filtrate is the waste water after handling, the active carbon reproducible utilization being obtained by filtration.
Embodiment 10
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；It is yellow to prepare 50mL 8mg/L ethyl
Drug solns are spare as the waste water containing xanthate；By weighed load TiO2Prepared ethyl xanthate solution is added in active carbon
In, its pH value is adjusted to 11 with 1mol/L NaOH solution, standing adsorption 60min；Suspension is obtained after standing, and to suspension mistake
Filter, obtains filtrate and active carbon after filtering, filtrate is the waste water after handling, the active carbon reproducible utilization being obtained by filtration.
Embodiment 11
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；Prepare 50mL 12mg/L ethyl
Xanthate solution is spare as the waste water containing xanthate；By weighed load TiO2It is molten that prepared ethyl xanthate is added in active carbon
In liquid, its pH value is adjusted to 11 with 1mol/L NaOH solution, standing adsorption 90min；Suspension is obtained after standing, and to suspension
Filtering, obtains filtrate and active carbon after filtering, filtrate is the waste water after handling, the active carbon reproducible utilization being obtained by filtration.
Embodiment 12
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared2Active carbon is used to adsorb useless containing xanthate
Water, adsorption method follow the steps below: weighing 0.03g load TiO2Active carbon, it is spare；Prepare 50mL 10mg/L ethyl
Xanthate solution is spare as the waste water containing xanthate；By weighed load TiO2It is molten that prepared ethyl xanthate is added in active carbon
In liquid, adjust its pH value to 11 with 1mol/L NaOH solution, respectively standing adsorption 10min, 30min, 50min, 70min and
90min；Suspension is obtained after standing, and suspension is imported in ionic tube and is centrifugated, and the supernatant after taking centrifuge separation is surveyed
Its fixed COD value, and calculate adsorption rate；Wherein, measurement reference standard GB11914 " the measurement weight chromium of water chemical oxygen demand of COD
Hydrochlorate method ".
Comparative example
0.03g active carbon is weighed, it is spare；Preparation 50mL 10mg/L ethyl xanthate solution is standby as the waste water containing xanthate
With；Weighed active carbon is added in prepared ethyl xanthate solution, adjusts its pH value to 11 with 1mol/L NaOH solution,
Standing adsorption 10min, 30min, 50min, 70min and 90min respectively；Obtain suspension after standing, and by suspension import from
It is centrifugated in sub- pipe, the supernatant after taking centrifuge separation measures its COD value, and calculates adsorption rate；Wherein, the measurement ginseng of COD
Examine standard GB11914 " the measurement dichromate titration of water chemical oxygen demand ".
The pH value of ethyl xanthate solution used in embodiment 12 and comparative example is 11, with Shaanxi shake prosperous mine difficult to understand
The waste water of industry Co., Ltd flotation is identical.
The concentration of ethyl xanthate and the functional relation of COD are COD=168.91+ in embodiment 12 and comparative example
2.61c1, c1For the concentration of ethyl xanthate.
The adsorption rate of xanthate in waste water is calculated according to the following formula in embodiment 12 and comparative example: R=(1-c/c0)×
100%；Wherein, R is adsorption rate, unit %；c0For the initial concentration of ethyl xanthate solution, unit mg/L；C is ethyl xanthate
The residual concentration of solution, unit mg/L.C in embodiment 6 and comparative example0For 10mg/L.
The test result of embodiment 12 and comparative example is shown in Fig. 1.As shown in Figure 1, when adsorption time is 10 minutes,
Active carbon is 50% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, and uses load TiO of the invention2Active carbon pair
The adsorption rate of ethyl xanthate is 71% in waste water containing xanthate, and compared with conventional activated carbon adsorption, adsorption rate is significantly improved
21%；When adsorption time is 30 minutes, active carbon is 54% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, and
Use load TiO of the invention2Active carbon is 77% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, with conventional work
Property charcoal absorption compare, adsorption rate significantly improves 23%；When adsorption time is 50 minutes, active carbon is to the waste water containing xanthate
The adsorption rate of middle ethyl xanthate is 57%, and uses load TiO of the invention2Active carbon is yellow to ethyl in the waste water containing xanthate
The adsorption rate of medicine is 80%, and compared with conventional activated carbon adsorption, adsorption rate significantly improves 23%；When adsorption time is 70 points
Zhong Shi, active carbon is 64% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, and uses load TiO of the invention2It is living
Property charcoal be 85% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, compared with conventional activated carbon adsorption, adsorption rate is aobvious
Work improves 21%；When adsorption time is 90 minutes, active carbon is to the adsorption rate of ethyl xanthate in the waste water containing xanthate
66%, and use load TiO of the invention2Active carbon is 86% to the adsorption rate of ethyl xanthate in the waste water containing xanthate, with
Conventional activated carbon adsorption is compared, and adsorption rate significantly improves 20%；Meanwhile under conditions of adsorption time is 90 minutes, knot
Ultraviolet light irradiation is closed, load TiO of the invention is used2Active carbon improves the adsorption rate of ethyl xanthate in the waste water containing xanthate
To 95%, the absorption of specific activity charcoal improves 29%；It is indicated above load TiO of the invention2Active carbon is remarkably improved alkalinity
Under the conditions of to the adsorption rate of xanthate in flotation waste water.
The load TiO for being used to adsorb xanthate that embodiment 1 is prepared of embodiment 7-112Active carbon contains for adsorbing
There is the waste water of xanthate, the adsorption effect of xanthate is obviously promoted compared with activated carbon adsorption, adsorption rate improves 20-
23%.
By prepared load TiO any in embodiment 2-62Active carbon is used to adsorb in the flotation waste water containing xanthate,
And compared with activated carbon adsorption, the load TiO of test result and the preparation of embodiment 12The absorption result of active carbon is consistent, absorption
Rate improves 20-23%.
The load TiO for being used to adsorb xanthate of the invention2Active carbon is to containing other types such as butyl xanthate, amyl group xanthate
The waste water of xanthate also has good suction-operated, and adsorption effect is suitable to the adsorption effect containing ethyl xanthate with it, with work
Property charcoal absorption compare, adsorption rate improve 20-23%, in conjunction with ultraviolet light, adsorption rate can promote 25% or more.
TiO2It is a kind of common catalyst, xanthate can be oxidized to CO under ultraviolet light irradiation by it2And other SO4 2-。
The present invention is by TiO2It is carried on the surface of active carbon, the huge specific surface area of active carbon on the one hand can be played, xanthate is adsorbed
In activated carbon surface, TiO on the other hand can be played2Catalytic action, xanthate is aoxidized, make activated carbon surface keep activity,
To extend the service life of active carbon.
In addition, the load TiO for being used to adsorb xanthate of the invention2Active carbon similarly has other collecting agents good
Adsorption effect.
Although the present invention is described in detail with a general description of the specific embodiments in this specification,
But on the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.
Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed model
It encloses.
Claims (6)
1. a kind of for adsorbing the load TiO of xanthate2Active carbon, which is characterized in that including following material composition: butyl titanate, nothing
Water-ethanol and active carbon；The ratio of the butyl titanate, dehydrated alcohol and the active carbon is (2-4) mL:(5-10) mL:1g；
The load TiO for being used to adsorb xanthate2The preparation method of active carbon, comprising the following steps:
Step 1, butyl titanate is mixed with dehydrated alcohol, stirs 15-30min under the speed of 400-600r/min, obtains yellow
Clear solution；
Step 2, the yellow transparent solution is added dropwise to HNO3In solution, after being added dropwise to complete, continue to stir 2-3h, and use NaOH
Solution adjusts pH to 1-2, and 20-30min is sufficiently stirred, obtains TiO2Colloidal sol；
Step 3, the TiO is added in active carbon2It in colloidal sol, stirs, is layered after standing, sediment is taken out, by sediment in 80-
It is dried under the conditions of 100 DEG C, and calcines 1-3h under the conditions of 400-500 DEG C to get load TiO2Active carbon；
Wherein, in step 2, the HNO3Solution is the mixing speed 800-1000r/min in stirring, described to drip
At time be 1-2h.
2. according to claim 1 for adsorbing the load TiO of xanthate2Active carbon, which is characterized in that described in step 3
The TiO is added in active carbon2Before in colloidal sol, the active carbon is added to the water infiltration 1-2h first.
3. according to claim 1 for adsorbing the load TiO of xanthate2Active carbon, which is characterized in that described in step 3
The time of stirring is 18-24h, and the speed of the stirring is 400-600r/min.
4. a kind of as described in claim 1 for adsorbing the load TiO of xanthate2The adsorption method of active carbon, which is characterized in that
It follows the steps below: by the load TiO for being used to adsorb xanthate2Active carbon is placed in the waste water containing xanthate, is stood
Absorption；The waste water containing xanthate is alkalinity.
5. according to claim 4 for adsorbing the load TiO of xanthate2The adsorption method of active carbon, which is characterized in that institute
State the load TiO for adsorbing xanthate2The ratio of adsorption of active carbon and the waste water containing xanthate is 0.03g:(30-50)
mL。
6. according to claim 5 for adsorbing the load TiO of xanthate2The adsorption method of active carbon, which is characterized in that institute
The concentration for stating the waste water containing xanthate is 8-12mg/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752268A (en) * | 2014-01-16 | 2014-04-30 | 广东工业大学 | Preparation method of filter core for adsorbing heavy metal, arsenic and fluorine in drinking water and application thereof |
| CN103803645A (en) * | 2014-02-19 | 2014-05-21 | 陕西科技大学 | Method for preparing anatase TiO2 nanometer hollow sphere |
| CN106423130A (en) * | 2016-09-21 | 2017-02-22 | 西安建筑科技大学 | Preparation and application of titanium dioxide/activated carbon self-assembled composite |
| CN106669591A (en) * | 2017-01-20 | 2017-05-17 | 贵州省材料产业技术研究院 | Treatment method for adsorbing xanthate in wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752268A (en) * | 2014-01-16 | 2014-04-30 | 广东工业大学 | Preparation method of filter core for adsorbing heavy metal, arsenic and fluorine in drinking water and application thereof |
| CN103803645A (en) * | 2014-02-19 | 2014-05-21 | 陕西科技大学 | Method for preparing anatase TiO2 nanometer hollow sphere |
| CN106423130A (en) * | 2016-09-21 | 2017-02-22 | 西安建筑科技大学 | Preparation and application of titanium dioxide/activated carbon self-assembled composite |
| CN106669591A (en) * | 2017-01-20 | 2017-05-17 | 贵州省材料产业技术研究院 | Treatment method for adsorbing xanthate in wastewater |
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