CN110152618A - A kind of heavy metal ion adsorbing material and preparation method thereof based on graphene - Google Patents
A kind of heavy metal ion adsorbing material and preparation method thereof based on graphene Download PDFInfo
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- CN110152618A CN110152618A CN201810263534.1A CN201810263534A CN110152618A CN 110152618 A CN110152618 A CN 110152618A CN 201810263534 A CN201810263534 A CN 201810263534A CN 110152618 A CN110152618 A CN 110152618A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention belongs to environment-friendly materials fields, more particularly to a kind of heavy metal ion adsorbing material and preparation method thereof based on graphene, raw material including following parts by weight: 60-100 parts of nitrogen-doped graphene, 10-30 parts of calcium carbonate, 20-50 parts of ethyl alcohol, 5-25 parts of medical stone, 20-40 parts of sepiolite, 15-35 parts of glycine, 1-5 parts of sodium nitrate, 6-10 parts of ammonium hydrogen carbonate, 2-6 parts of titanium dioxide, 3-7 parts of methylcellulose, 12-18 parts of talcum powder, 5-9 parts of initiator, 12-19 parts of crosslinking agent, 70-130 parts of deionized water.A kind of this clearly demarcated heavy metal ion adsorbing material and preparation method thereof based on graphene, it is low in cost, the rate of adsorption is fast, adsorption capacity is big；Sea bubble mud adsorption capacity is strong；Nitrogen-doped graphene is enhancing heavy metal ion adsorbing material；Heavy metal ion adsorbing material of the invention can also carry out rapid regeneration by alkalinity potassium permanganate.
Description
Technical field
The invention belongs to environment-friendly materials fields, and in particular to a kind of heavy metal ion adsorbing material based on graphene and its
Preparation method.
Background technique
In recent years, environmental pollution is of increasing concern, and the removing of heavy metal ions in sewage becomes hot research, main
Processing method includes absorption method, chemical precipitation method, ion-exchange, membrane separation process, bio-flocculation process etc., wherein absorption method tool
There is the advantages that easy to operate, heavy metal treatment effect is preferable.
Absorption method is the active site surface for making heavy metal ion be adhered to adsorbent by physics and chemical method, into
And reaching the method for heavy-metal ion removal purpose, common adsorbent includes natural material and two kinds of artificial material, natural material
Material includes active carbon, minerals, agriculture and forestry organic waste material, silt etc., and artificial material includes nano material etc., in general, natural material
Material transaction obtains, and cost is relatively low, but adsorption effect is poor, and artificial material preparation cost is high and natural material, but adsorption effect compared with
It is good.
Summary of the invention
The purpose of the present invention is to provide a kind of heavy metal ion adsorbing material and preparation method thereof based on graphene, at
This is cheap, the rate of adsorption is fast, adsorption capacity is big.
A kind of heavy metal ion adsorbing material based on graphene, the raw material including following parts by weight:
60-100 parts of nitrogen-doped graphene, 10-30 parts of calcium carbonate, 20-50 parts of ethyl alcohol, 5-25 parts of medical stone, sepiolite 20-40
Part, it is 15-35 parts of glycine, 1-5 parts of sodium nitrate, 6-10 parts of ammonium hydrogen carbonate, 2-6 parts of titanium dioxide, 3-7 parts of methylcellulose, sliding
12-18 parts of mountain flour, 5-9 parts of initiator, 12-19 parts of crosslinking agent, 70-130 parts of deionized water.
The initiator is any one in benzoyl peroxide and lauroyl peroxide, and the crosslinking agent is double methyl-props
Any one in olefin(e) acid glycol ester and divinylbenzene.
The preparation method of the heavy metal ion adsorbing material based on graphene, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 30-
After sixty minutes, step (1) products therefrom is added, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；
(4) step (3) described product filtered, washed, 60-70 DEG C of drying；
(5) step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to
The heavy metal ion adsorbing material based on graphene is made in constant weight.
Heating temperature is 85-95 DEG C in the step (3), and mixing time is 4-8 hours, mixing speed 55-65rpm.
Alkalinity potassium permanganate in the step (5) the preparation method comprises the following steps: the permanganic acid for being 5-10% to 1L mass fraction
The sodium hydroxide of 0.05-0.1mol is added in potassium solution.
The invention has the following advantages: a kind of this clearly demarcated heavy metal ion adsorbing material based on graphene and its
Preparation method, it is low in cost, the rate of adsorption is fast, adsorption capacity is big；Sea bubble mud adsorption capacity is strong；Nitrogen-doped graphene is enhancing weight
Metal ion adsorption material；Heavy metal ion adsorbing material of the invention can also carry out rapid regeneration by alkalinity potassium permanganate.
Specific embodiment
Embodiment 1
A kind of heavy metal ion adsorbing material based on graphene, the raw material including following parts by weight:
60 parts of nitrogen-doped graphene, 10 parts of calcium carbonate, 20 parts of ethyl alcohol, 5 parts of medical stone, 20 parts of sepiolite, 15 parts of glycine, nitric acid
1 part of sodium, 6 parts of ammonium hydrogen carbonate, 2 parts of titanium dioxide, 3 parts of methylcellulose, 12 parts of talcum powder, 5 parts of initiator, 12 parts of crosslinking agent,
Deionized water 70.
Wherein initiator is benzoyl peroxide, and crosslinking agent is ethyleneglycol dimethyacrylate.
The preparation method of the heavy metal ion adsorbing material based on graphene, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 30 divides
Zhong Hou is added step (1) products therefrom, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；Heating temperature is 85 DEG C；Mixing time
It is 4 hours；Mixing speed is 55rpm.
(4) step (3) described product filtered, washed, 60 DEG C of drying；
(5) sodium hydroxide of 0.05mol is added into the liquor potassic permanganate of 1L 5%, and that 5% alkalinity potassium permanganate is prepared is molten
Liquid；Step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to perseverance
The heavy metal ion adsorbing material based on graphene is made in weight.
Embodiment 2
A kind of heavy metal ion adsorbing material based on graphene, the raw material including following parts by weight:
100 parts of nitrogen-doped graphene, 30 parts of calcium carbonate, 50 parts of ethyl alcohol, 25 parts of medical stone, 40 parts of sepiolite, 35 parts of glycine, nitre
5 parts of sour sodium, 10 parts of ammonium hydrogen carbonate, 6 parts of titanium dioxide, 7 parts of methylcellulose, 18 parts of talcum powder, 9 parts of initiator, crosslinking agent 19
Part, deionized water 130.
Wherein initiator is lauroyl peroxide, and crosslinking agent is divinylbenzene.
The preparation method of the heavy metal ion adsorbing material based on graphene, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 60 divides
Zhong Hou is added step (1) products therefrom, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；Heating temperature is 95 DEG C；Mixing time
It is 8 hours；Mixing speed is 65rpm.
(4) step (3) described product filtered, washed, 70 DEG C of drying；
(5) sodium hydroxide of 0.1mol is added into the liquor potassic permanganate of 1L 10%, and that 10% alkalinity potassium permanganate is prepared is molten
Liquid；Step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to perseverance
The heavy metal ion adsorbing material based on graphene is made in weight.
Embodiment 3
A kind of heavy metal ion adsorbing material based on graphene, the raw material including following parts by weight:
65 parts of nitrogen-doped graphene, 15 parts of calcium carbonate, 25 parts of ethyl alcohol, 7 parts of medical stone, 25 parts of sepiolite, 20 parts of glycine, nitric acid
3 parts of sodium, 8 parts of ammonium hydrogen carbonate, 4 parts of titanium dioxide, 5 parts of methylcellulose, 14 parts of talcum powder, 7 parts of initiator, 14 parts of crosslinking agent,
Deionized water 80.
Wherein initiator is benzoyl peroxide, and crosslinking agent is divinylbenzene.
The preparation method of the heavy metal ion adsorbing material based on graphene, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 40 divides
Zhong Hou is added step (1) products therefrom, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；Heating temperature is 87 DEG C；Mixing time
It is 6 hours；Mixing speed is 58rpm.
(4) step (3) described product filtered, washed, 65 DEG C of drying；
(5) sodium hydroxide of 0.06mol is added into the liquor potassic permanganate of 1L 7%, and that 7% alkalinity potassium permanganate is prepared is molten
Liquid；Step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to perseverance
The heavy metal ion adsorbing material based on graphene is made in weight.
Embodiment 4
A kind of heavy metal ion adsorbing material based on graphene, the raw material including following parts by weight:
90 parts of nitrogen-doped graphene, 28 parts of calcium carbonate, 45 parts of ethyl alcohol, 20 parts of medical stone, 35 parts of sepiolite, 30 parts of glycine, nitre
4 parts of sour sodium, 8 parts of ammonium hydrogen carbonate, 5 parts of titanium dioxide, 5 parts of methylcellulose, 16 parts of talcum powder, 7 parts of initiator, crosslinking agent 17
Part, deionized water 100.
Wherein initiator is lauroyl peroxide, and crosslinking agent is ethyleneglycol dimethyacrylate.
The preparation method of the heavy metal ion adsorbing material based on graphene, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 50 divides
Zhong Hou is added step (1) products therefrom, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；Heating temperature is 90 DEG C；Mixing time
It is 7 hours；Mixing speed is 60rpm.
(4) step (3) described product filtered, washed, 65 DEG C of drying；
(5) sodium hydroxide of 0.08mol is added into the liquor potassic permanganate of 1L 8%, and that 8% alkalinity potassium permanganate is prepared is molten
Liquid；Step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to perseverance
The heavy metal ion adsorbing material based on graphene is made in weight.
Claims (5)
1. a kind of heavy metal ion adsorbing material based on graphene, which is characterized in that the raw material including following parts by weight:
60-100 parts of nitrogen-doped graphene, 10-30 parts of calcium carbonate, 20-50 parts of ethyl alcohol, 5-25 parts of medical stone, sepiolite 20-40
Part, it is 15-35 parts of glycine, 1-5 parts of sodium nitrate, 6-10 parts of ammonium hydrogen carbonate, 2-6 parts of titanium dioxide, 3-7 parts of methylcellulose, sliding
12-18 parts of mountain flour, 5-9 parts of initiator, 12-19 parts of crosslinking agent, 70-130 parts of deionized water.
2. a kind of heavy metal ion adsorbing material based on graphene according to claim 1, which is characterized in that described to draw
Sending out agent is any one in benzoyl peroxide and lauroyl peroxide, the crosslinking agent be ethyleneglycol dimethyacrylate and
Any one in divinylbenzene.
3. the preparation method of the heavy metal ion adsorbing material according to claim 1 or described in 2 any one based on graphene,
It is characterized in that, comprising the following steps:
(1) ethyl alcohol, glycine, sodium nitrate, ammonium hydrogen carbonate, titanium dioxide and methylcellulose investment are equipped with blender and temperature
In the reaction kettle of meter, 60 DEG C are warming up to, stirs 30min, mixing speed is 800 revs/min；
(2) nitrogen-doped graphene, calcium carbonate, medical stone, sepiolite and talcum powder are mixed with deionized water, ultrasonic disperse 30-
After sixty minutes, step (1) products therefrom is added, is uniformly mixed；
(3) initiator and crosslinking agent, heating stirring are added into step (2) acquired solution；
(4) step (3) described product filtered, washed, 60-70 DEG C of drying；
(5) step (4) described product is placed in alkaline permanganate solution after being soaked for a period of time, filters, washs, is dried to
The heavy metal ion adsorbing material based on graphene is made in constant weight.
4. the preparation method of the heavy metal ion adsorbing material according to claim 3 based on graphene, which is characterized in that
Heating temperature is 85-95 DEG C in the step (3), and mixing time is 4-8 hours, mixing speed 55-65rpm.
5. the preparation method of the heavy metal ion adsorbing material according to claim 3 based on graphene, which is characterized in that
Alkalinity potassium permanganate in the step (5) the preparation method comprises the following steps: in the liquor potassic permanganate for being 5-10% to 1L mass fraction
The sodium hydroxide of 0.05-0.1mol is added.
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Application publication date: 20190823 |