CN109174058A - The preparation method of secondary chlorine white clay adsorbing material for depth removal complex state chromium - Google Patents
The preparation method of secondary chlorine white clay adsorbing material for depth removal complex state chromium Download PDFInfo
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- 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
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- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- 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
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- C02F1/00—Treatment of water, waste water, or sewage
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- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C02F2103/22—Nature of the water, waste water, sewage or sludge to be treated from the processing of animals, e.g. poultry, fish, or parts thereof
- C02F2103/24—Nature of the water, waste water, sewage or sludge to be treated from the processing of animals, e.g. poultry, fish, or parts thereof from tanneries
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention belongs to solid waste resource utilization field more particularly to a kind of preparation methods of the secondary chlorine white clay adsorbing material for depth removal complex state chromium, implement as follows: (1) secondary chlorine white clay is dry to constant weight, it is ground up, sieved, acidleach, filtering, obtains filtrate；(2) cetyl trimethylammonium bromide, ultrasonic disperse is added into step (1) described filtrate；Add ethylenediamine tetra-acetic acid；(3) conductive graphene dispersion liquid is added in ethanol solution, ultrasonic disperse；Under agitation, it is added in step (2) products therefrom and stirs, ball milling；(4) graphene oxide dispersion is added into step (3) products therefrom, continues ultrasonic disperse；(5) liquid obtained by step (4) is centrifuged, spray drying, air-flow crushing is to get purpose product time chlorine white clay adsorbing material.Operation of the present invention is simple, and purpose product complex state chromium adsorption rate is high, can effectively solve time chlorine white mud waste residue.
Description
Technical field
The invention belongs to solid waste resource utilization field more particularly to a kind of times for depth removal complex state chromium
The preparation method of chlorine white clay adsorbing material.
Background technique
Currently, the production technology of titanium dioxide only has sulfuric acid process and two kinds of chloridising, but the two finished product price produced
Differ many thousands of (per ton).The titanium dioxide of Production By Sulfuric Acid Process is not only worth low, but also purposes is narrow.Chloridising production has the three wastes
Less, good product quality and the advantages that controllable uniform particle sizes.Titanium Dioxide Produced by Chloride Procedure production procedure mainly divides 3 parts: chlorination, oxidation and
Treatment and finishing section.Secondary chlorine white clay is the solidliquid mixture generated after the tail gas alkali of chloridization process elutes, by precipitating, plate compression
Afterwards, the solid of formation.Industry is deposited in on-site at present, can not be disposed.Therefore, the secondary chlorine white clay generated for chloridising
The technology that waste residue is effectively disposed urgently is promoted.
Secondary chlorine white clay is mainly with Ti, TiO2, the components such as Mn, V, Ca, Fe, Al constitute, Compound Heavy Metals absorption can be prepared and received
Rice functional material.Graphene has high specific surface area, heating conduction outstanding, high electron mobility, good chemistry steady
Qualitative and excellent mechanical property etc. is widely used in many fields.In recent years, both at home and abroad gradually by graphite
Alkene is used as adsorbent material, but graphene is easy to reunite, thus can prepare nano material and graphene is compound to improve its performance.Oxidation
Graphene surface contains the groups such as carbonyl, hydroxyl, carboxyl, so that it has good hydrophily, and oxygen-containing group can be with
Metal ion is had an effect, and then can be with the metal ion in separation and concentration water phase.
Summary of the invention
The present invention is directed to a kind of easy to operate, low in cost, purpose product is provided in place of overcome the deficiencies in the prior art
Complex state chromium adsorption rate is high, can effectively solve the secondary chlorine white clay base absorption for depth removal complex state chromium of time chlorine white mud waste residue
The preparation method of material.
In order to solve the above technical problems, the invention is realized in this way.
A kind of preparation method of the secondary chlorine white clay adsorbing material for depth removal complex state chromium, it is real as follows
It applies:
(1) secondary chlorine white clay is dry to constant weight, it is ground up, sieved, acidleach, filters, obtain filtrate；
(2) under agitation, cetyl trimethylammonium bromide, ultrasonic disperse is added into step (1) described filtrate；Again plus
Enter ethylenediamine tetra-acetic acid；
(3) conductive graphene dispersion liquid is added in ethanol solution, ultrasonic disperse；Under agitation, step (2) are added to
It is stirred in products therefrom, ball milling；
(4) under agitation, graphene oxide dispersion is added into step (3) products therefrom, continues ultrasonic disperse；
(5) liquid obtained by step (4) is centrifuged, spray drying, air-flow crushing is to get purpose product time chlorine white clay base adsorption material
Material.
As a preferred embodiment, in the step (1) of the present invention, secondary chlorine white clay is dried at 60 DEG C to constant weight, grinding
Be sieved 100~1000 mesh；And its 100g is taken to be added in the sulfuric acid of 200mL mass concentration 10~20%, and 2~4h of acidleach, filtering,
Obtain filtrate.
Further, in step (2) of the present invention, under agitation, into step (1) described filtrate be added 6~
10g cetyl trimethylammonium bromide, 30~60min of ultrasonic disperse；Add ethylenediamine tetra-acetic acid；Cetyl trimethyl bromine
Change 2~10:5 of mass ratio of ammonium and ethylenediamine tetra-acetic acid.
Further, in step (3) of the present invention, 0.2g~1.0g conductive graphene dispersion liquid is added to 200ml
In ethanol solution, 30~60min of ultrasonic disperse；Under agitation, it is added in step (2) products therefrom, stirring 30~
Ball milling pearl ball milling is added in 60min.
Further, in step (4) of the present invention, under agitation, by conductive graphene and graphene oxide matter
Graphene oxide dispersion is added into step (3) products therefrom than 1:1~5 for amount, continues 30~60min of ultrasonic disperse.
Further, in step (3) of the present invention, conductive graphene dispersion liquid concentration 5mg/ml, piece diameter 10nm~2 μ
M, 1000~1800S/cm of conductivity.
Further, in step (3) of the present invention, ball milling bead diameter that ball milling uses is 50~200 μm, ball milling speed
100~500r/min, 30~150min of Ball-milling Time.
The invention has the advantages that
(1) present invention realizes waste resource recovery utilization using time chlorine white mud waste residue as raw material, at low cost, solves industry
Upper waste residue intractable problem, reduces environmental pollution；
(2) contain Ti, TiO in the secondary chlorine white mud waste residue that the present invention uses2Equal ingredients, by acidleach, the means such as ultrasonic disperse are real
Show compound with graphene, its absorption property can be improved；Pass through the adsorption test to the complex state chromium in waste water, it was demonstrated that this hair
The secondary chlorine white clay adsorbing material adsorbance with higher and removal rate of bright preparation；
(3) of the invention easy to operate, it is convenient for industrial applications, economic benefit and social benefit are all fairly obvious.
Secondary chlorine white clay adsorbing material prepared by the present invention has that removal rate is high, absorption property is excellent, cheap etc. excellent
Point, can be widely used for leather waste water, in dyeing waste water heavy metal and organic pollutant removal.
Specific embodiment
The present invention is further explained in the light of specific embodiments.Protection scope of the present invention is not only limited to following
The statement of content.
Embodiment:
(1) secondary chlorine white clay is dried at 60 DEG C to constant weight, is ground up, sieved 100 mesh；And its 100g is taken to be added to 200mL mass concentration
10% sulfuric acid (H2SO4) in, acidleach 2h, filtering obtains filtrate；
(2) under agitation, cetyl trimethylammonium bromide (CTAB) 6g, ultrasonic disperse is added in filtrate in step (1)
30min；Ethylenediamine tetra-acetic acid (EDTA) is added, according to mass ratio (CTAB:EDTA) 2:5；
(3) conductive graphene dispersion liquid (concentration 5mg/ml, conductive graphene piece diameter 10nm, conductivity 1000S/cm) 0.2g is added
Enter into 200ml ethanol solution, ultrasonic disperse 30min；Under agitation, it is added in step (2) products therefrom, high-speed stirring
30min is mixed, is added ball milling pearl ball milling (50 μm of ball milling bead diameter, ball milling speed 100r/min, Ball-milling Time 30min)；
(4) under agitation, (conductive graphene and graphene oxide) 1:1 in mass ratio adds into step (3) products therefrom
Enter graphene oxide dispersion (concentration 5mg/ml, graphene oxide sheet diameter 10nm), continues ultrasonic disperse 30min；
(5) liquid in step (4) is centrifuged, is spray-dried, air-flow crushing, obtain time chlorine white clay adsorbing material.
Six hydrated sulfuric acid chromium are used to prepare total chromium concn as the solution of 5~30mg/L, preferably total chromium concn is 20mg/L, is pressed
Formic acid (FA) and Cr (III) molar ratio are that 1:1 configures FA-Cr complex liquid, adjust pH value of solution=4~6 FA-Cr, respectively take 50mLFA-Cr
Complex liquid is fitted into 4 250mL conical flasks, and secondary chlorine white clay adsorbing material additional amount is 1g, number 1,2,3,4, No. 1 conduct
Control group at the uniform velocity stirs at 40 DEG C, adsorption time 90min, static 5min, and is centrifuged 10min with 3000r/min, takes
Clear liquid surveys total chromium concn.
Embodiment 2:
(1) secondary chlorine white clay is dried at 60 DEG C to constant weight, is ground up, sieved 200 mesh；And its 100g is taken to be added to 200mL mass concentration
10% sulfuric acid (H2SO4) in, acidleach 2h, filtering obtains filtrate；
(2) under agitation, cetyl trimethylammonium bromide (CTAB) 7g, ultrasonic disperse is added in filtrate in step (1)
30min；Ethylenediamine tetra-acetic acid (EDTA) is added, according to mass ratio (CTAB:EDTA) 4:5；
(3) conductive graphene dispersion liquid (concentration 5mg/ml, conductive graphene piece diameter 10nm, conductivity 1000S/cm) 0.4g is added
Enter into 200ml ethanol solution, ultrasonic disperse 30min；Under agitation, it is added in step (2) products therefrom, high-speed stirring
30min is mixed, is added ball milling pearl ball milling (50 μm of ball milling bead diameter, ball milling speed 200r/min, Ball-milling Time 60min)；
(4) under agitation, (conductive graphene and graphene oxide) 1:2 in mass ratio adds into step (3) products therefrom
Enter graphene oxide dispersion (concentration 5mg/ml, graphene oxide sheet diameter 10nm), continues ultrasonic disperse 30min；
(5) liquid in step (4) is centrifuged, is spray-dried, air-flow crushing, obtain time chlorine white clay adsorbing material.
Six hydrated sulfuric acid chromium are used to prepare total chromium concn as the solution of 5~30mg/L, preferably total chromium concn is 20mg/L, is pressed
Formic acid (FA) and Cr (III) molar ratio are that 1:1 configures FA-Cr complex liquid, adjust pH value of solution=4~6 FA-Cr, respectively take 50mLFA-Cr
Complex liquid is fitted into 4 250mL conical flasks, secondary chlorine white clay adsorbing material additional amount 1g, number 1,2,3,4, No. 1 conduct pair
It is at the uniform velocity stirred at 40 DEG C according to group, adsorption time 90min, static 5min, and 10min is centrifuged with 3000r/min, take supernatant
Liquid surveys total chromium concn.
Embodiment 3:
(1) secondary chlorine white clay is dried at 60 DEG C to constant weight, is ground up, sieved 300 mesh；And its 100g is taken to be added to 200mL mass concentration
20% sulfuric acid (H2SO4) in, acidleach 4h, filtering obtains filtrate；
(2) under agitation, cetyl trimethylammonium bromide (CTAB) 8g, ultrasonic disperse is added in filtrate in step (1)
60min；Ethylenediamine tetra-acetic acid (EDTA) is added, according to mass ratio (CTAB:EDTA) 6:5；
(3) conductive graphene dispersion liquid (concentration 5mg/ml, 1 μm of conductive graphene piece diameter, conductivity 1200S/cm) 0.6g is added
Enter into 200ml ethanol solution, ultrasonic disperse 60min；Under agitation, it is added in step (2) products therefrom, high-speed stirring
60min is mixed, is added ball milling pearl ball milling (100 μm of ball milling bead diameter, ball milling speed 300r/min, Ball-milling Time 90min)；
(4) under agitation, (conductive graphene and graphene oxide) 1:3 in mass ratio adds into step (3) products therefrom
Enter graphene oxide dispersion (concentration 5mg/ml, 1 μm of conductive graphene piece diameter), continues ultrasonic disperse 60min；
(5) liquid in step (4) is centrifuged, is spray-dried, air-flow crushing, obtain time chlorine white clay adsorbing material.
Six hydrated sulfuric acid chromium are used to prepare total chromium concn as the solution of 5~30mg/L, preferably total chromium concn is 20mg/L, is pressed
Formic acid (FA) and Cr (III) molar ratio are that 1:1 configures FA-Cr complex liquid, adjust pH value of solution=4~6 FA-Cr, respectively take 50mLFA-Cr
Complex liquid is fitted into 4 250mL conical flasks, secondary chlorine white clay adsorbing material additional amount 1g, number 1,2,3,4, No. 1 conduct pair
It is at the uniform velocity stirred at 40 DEG C according to group, adsorption time 90min, static 5min, and 10min is centrifuged with 3000r/min, take supernatant
Liquid surveys total chromium concn.
Embodiment 4:
(1) secondary chlorine white clay is dried at 60 DEG C to constant weight, is ground up, sieved 400 mesh；And its 100g is taken to be added to 200mL mass concentration
20% sulfuric acid (H2SO4) in, acidleach 4h, filtering obtains filtrate；
(2) under agitation, cetyl trimethylammonium bromide (CTAB) 9g, ultrasonic disperse is added in filtrate in step (1)
60min；Ethylenediamine tetra-acetic acid (EDTA) is added, according to mass ratio (CTAB:EDTA) 8:5；
(3) conductive graphene dispersion liquid (concentration 5mg/ml, 1 μm of conductive graphene piece diameter, conductivity 1200S/cm) 0.8g is added
Enter into 200ml ethanol solution, ultrasonic disperse 60min；Under agitation, it is added in step (2) products therefrom, high-speed stirring
60min is mixed, is added ball milling pearl ball milling (100 μm of ball milling bead diameter, ball milling speed 400r/min, Ball-milling Time 120min)；
(4) under agitation, (conductive graphene and graphene oxide) 1:4 in mass ratio adds into step (3) products therefrom
Enter graphene oxide dispersion (concentration 5mg/ml, 1 μm of conductive graphene piece diameter), continues ultrasonic disperse 60min；
(5) liquid in step (4) is centrifuged, is spray-dried, air-flow crushing, obtain time chlorine white clay adsorbing material.
Six hydrated sulfuric acid chromium are used to prepare total chromium concn as the solution of 5~30mg/L, preferably total chromium concn is 20mg/L, is pressed
Formic acid (FA) and Cr (III) molar ratio are that 1:1 configures FA-Cr complex liquid, adjust pH value of solution=4~6 FA-Cr, respectively take 50mLFA-Cr
Complex liquid is fitted into 4 250mL conical flasks, secondary chlorine white clay adsorbing material additional amount 1g, number 1,2,3,4, No. 1 conduct pair
It is at the uniform velocity stirred at 40 DEG C according to group, adsorption time 90min, static 5min, and 10min is centrifuged with 3000r/min, take supernatant
Liquid surveys total chromium concn.
Embodiment 5:
(1) secondary chlorine white clay is dried at 60 DEG C to constant weight, is ground up, sieved 500 mesh；And its 100g is taken to be added to 200mL mass concentration
20% sulfuric acid (H2SO4) in, acidleach 4h, filtering obtains filtrate；
(2) under agitation, cetyl trimethylammonium bromide (CTAB) 10g, ultrasonic disperse is added in filtrate in step (1)
60min；Ethylenediamine tetra-acetic acid (EDTA) is added, according to mass ratio (CTAB:EDTA) 10:5；
(3) conductive graphene dispersion liquid (concentration 5mg/ml, 2 μm of conductive graphene piece diameter, conductivity 1800S/cm) 1.0g is added
Enter into 200ml ethanol solution, ultrasonic disperse 60min；Under agitation, it is added in step (2) products therefrom, high-speed stirring
60min is mixed, is added ball milling pearl ball milling (200 μm of ball milling bead diameter, ball milling speed 500r/min, Ball-milling Time 150min)；
(4) under agitation, (conductive graphene and graphene oxide) 1:5 in mass ratio adds into step (3) products therefrom
Enter graphene oxide dispersion (concentration 5mg/ml, 2 μm of conductive graphene piece diameter), continues ultrasonic disperse 60min；
(5) liquid in step (4) is centrifuged, is spray-dried, air-flow crushing, obtain time chlorine white clay adsorbing material.
Six hydrated sulfuric acid chromium are used to prepare total chromium concn as the solution of 5~30mg/L, preferably total chromium concn is 20mg/L, is pressed
Formic acid (FA) and Cr (III) molar ratio are that 1:1 configures FA-Cr complex liquid, adjust pH value of solution=4~6 FA-Cr, respectively take 50mLFA-Cr
Complex liquid is fitted into 4 250mL conical flasks, secondary chlorine white clay adsorbing material additional amount 1g, number 1,2,3,4, No. 1 conduct pair
It is at the uniform velocity stirred at 40 DEG C according to group, adsorption time 90min, static 5min, and 10min is centrifuged with 3000r/min, take supernatant
Liquid surveys total chromium concn.
Experimental data
The adsorbance (1) of secondary chlorine white clay adsorbing material prepared by Example 1~5 to complex state chromium, removal rate (2), formula
It is as follows:
Wherein:ηThe removal rate of-FA-Cr complex liquid, %；
C0The initial concentration of-FA-Cr complex liquid, mg/L；
Ct- FA-Cr complex liquid be adsorbed after concentration, mg/L；
qtThe adsorbance of-FA-Cr complex liquid, mg/g；
The volume of V-FA-Cr complex liquid, mL；
The quality of m- chlorine white clay adsorbing material, g.Its adsorbance result such as table 1, removal rate result such as table 2.
Adsorbance of time chlorine white clay adsorbing material to complex state chromium made from 1 Examples 1 to 5 of table.
Removal rate of time chlorine white clay adsorbing material to complex state chromium made from 2 Examples 1 to 5 of table.
It is to be understood that being merely to illustrate the present invention above with respect to specific descriptions of the invention and being not limited to this
Technical solution described in inventive embodiments, those skilled in the art should understand that, still the present invention can be carried out
Modification or equivalent replacement, to reach identical technical effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (7)
1. a kind of preparation method of the secondary chlorine white clay adsorbing material for depth removal complex state chromium, which is characterized in that by such as
Lower step is implemented:
(1) secondary chlorine white clay is dry to constant weight, it is ground up, sieved, acidleach, filters, obtain filtrate；
(2) under agitation, cetyl trimethylammonium bromide, ultrasonic disperse is added into step (1) described filtrate；Again plus
Enter ethylenediamine tetra-acetic acid；
(3) conductive graphene dispersion liquid is added in ethanol solution, ultrasonic disperse；Under agitation, step (2) are added to
It is stirred in products therefrom, ball milling；
(4) under agitation, graphene oxide dispersion is added into step (3) products therefrom, continues ultrasonic disperse；
(5) liquid obtained by step (4) is centrifuged, spray drying, air-flow crushing is to get purpose product time chlorine white clay base adsorption material
Material.
2. the preparation method of the secondary chlorine white clay adsorbing material according to claim 1 for depth removal complex state chromium,
It is characterized by: secondary chlorine white clay is dried at 60 DEG C to constant weight in the step (1), it is ground up, sieved 100~1000 mesh；And it takes
Its 100g is added in the sulfuric acid of 200mL mass concentration 10~20%, 2~4h of acidleach, and filtering obtains filtrate.
3. the preparation method of the secondary chlorine white clay adsorbing material according to claim 2 for depth removal complex state chromium,
It is characterized by: under agitation, 6~10g cetyl three is added into step (1) described filtrate in the step (2)
Methyl bromide ammonium, 30~60min of ultrasonic disperse；Add ethylenediamine tetra-acetic acid；Cetyl trimethylammonium bromide and ethylenediamine
2~10:5 of mass ratio of tetraacethyl.
4. the preparation method of the secondary chlorine white clay adsorbing material according to claim 3 for depth removal complex state chromium,
It is characterized by: 0.2g~1.0g conductive graphene dispersion liquid is added in 200ml ethanol solution in the step (3), surpass
Sound disperses 30~60min；Under agitation, it is added in step (2) products therefrom, stirs 30~60min, ball milling pearl is added
Ball milling.
5. the preparation method of the secondary chlorine white clay adsorbing material according to claim 4 for depth removal complex state chromium,
It is characterized by: in the step (4), under agitation, by conductive graphene and graphene oxide mass ratio 1:1~5 to
Graphene oxide dispersion is added in step (3) products therefrom, continues 30~60min of ultrasonic disperse.
6. the system of any secondary chlorine white clay adsorbing material for depth removal complex state chromium according to claim 1~5
Preparation Method, it is characterised in that: in the step (3), conductive graphene dispersion liquid concentration 5mg/ml, piece diameter 10nm~2 μm, conduction
1000~1800S/cm of rate.
7. the preparation method of the secondary chlorine white clay adsorbing material according to claim 6 for depth removal complex state chromium,
It is characterized by: in the step (3), ball milling bead diameter that ball milling uses is 50~200 μm, 100~500r/ of ball milling speed
Min, 30~150min of Ball-milling Time.
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|---|---|---|---|---|
| CN104692510A (en) * | 2015-04-02 | 2015-06-10 | 湖南科技大学 | Preparation method for solid polymer ferric sulfate zinc flocculant |
| CN105866212A (en) * | 2016-05-26 | 2016-08-17 | 江西农业大学 | Electrochemical sensor for detecting mercury ions and copper ions selectively and simultaneously and preparation method thereof |
| CN107670642A (en) * | 2017-11-23 | 2018-02-09 | 成都新柯力化工科技有限公司 | A kind of layered double hydroxide microballoon and preparation method for being used to handle sewage |
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