CN109126723A - A kind of preparation method and applications of the fly ash base adsorbent material of hydroxyl are administered in nickel contamination - Google Patents
A kind of preparation method and applications of the fly ash base adsorbent material of hydroxyl are administered in nickel contamination Download PDFInfo
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- CN109126723A CN109126723A CN201811068994.5A CN201811068994A CN109126723A CN 109126723 A CN109126723 A CN 109126723A CN 201811068994 A CN201811068994 A CN 201811068994A CN 109126723 A CN109126723 A CN 109126723A
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/041—Oxides or hydroxides
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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
- B01J20/06—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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- 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
- B01J20/06—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
- B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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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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- 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
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
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- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
A kind of preparation method and applications of the fly ash base adsorbent material of hydroxyl are administered in nickel contamination, belong to fly ash base adsorbent material technical field, environmental pollution caused by can solving the problems, such as existing undesirable the treatment effect of nickel and flyash, the preparation method is as follows: after mixing by acrylic acid, diethanol amine and ethylene glycol, the concentrated sulfuric acid is added, is heated to reflux；After acquired solution is neutralized, acrylamide is added, is uniformly mixed, is passed through nitrogen at room temperature, adds sodium hydrogensulfite and ammonium persulfate reaction；Flyash is added in above-mentioned solution, is stirred continuously, the reaction was continued；By the washing of gained mixture, drying, fly ash base adsorbent material is obtained.Flyash used in the present invention is a kind of solid waste, from a wealth of sources, and this law can both turn waste into wealth, and comprehensive utilization waste coal ash reduces environmental pollution, and can remove water pollutant Ni2+, effectively solve heavy metal nickel pollution problem.
Description
Technical field
The invention belongs to fly ash base adsorbent material technical fields, and in particular to a kind of fly ash base adsorption material of hydroxyl
The preparation method and applications of material are administered in nickel contamination.
Background technique
Average abundance of the nickel in the earth's crust is 75ppm, is comparision contents element abundant in microelement.The whole world is every
The migration situation of year nickel is: rock weathering amount is 320000 tons, and river conveying capacity is 19000 tons, and yield is 560000 tons, mine
Object fuel combustion discharges 5600 tons.At present, it is believed that nickel is a kind of potentially hazardous object to environment.Industrial major part nickel is used for
Manufacture stainless steel and corrosion-resisant alloy, and be widely used in nickel plating, coin, manufacture catalyst and glass ceramics etc..
Nickel plating industry, machine-building, metal-processing industry waste water in often contain nickel, commonly use alkaline process processing, make its generation
Nickel hydroxide (Ni (OH)2) precipitate and dispose.Nickel can be concentrated in the soil, nickeliferous Atmospheric particulates sedimentation, nickel-containing waste water
Irrigation, the rotten, rock weathering of plant and animal residues etc. are all the sources of nickel in soil.Plant growth can absorb the nickel in soil.Nickel
The highest plant of content is green vegetables and tobacco, up to 1.5-3ppm.Nickel to rice generate toxicity critical concentration be
20ppm.China provides that the maximum permissible concentration of carbonyl nickel in workshop air is 0.001mg/m3, the highest of nickel is allowed in the surface water
Concentration is 0.5mg/L.
Flyash is a kind of one of maximum solid industrial waste of thermal power plant discharge amount, is caused seriously to environment
Pollution.According to statistics, the main oxides composition of power plants flyash is respectively as follows: SiO2、Al2O3、TFeO(FeO+Fe2O3)、
CaO、TiO2、MgO、K2O、Na2O、SO3, MnO etc., wherein SiO2、Al2O3、TFeO(FeO+Fe2O3), tetra- kinds of component institute accountings of CaO
Example nearly 90%.The presence of these elements, making flyash not only has biggish surface area, but also is easy to carry out grafting modification.Utilize fine coal
The two advantages in grey structure prepare highly selective adsorbent material to be modified, and can not only reduce nickel contamination, and
And flyash can be carried out to resource utilization, reduce environmental pollution.Therefore, the present invention provides a kind of fly ash base adsorbent material
Preparation method and its remove water in Ni2+Application method, go water removal in Ni2+Aspect achieves excellent performance.
Summary of the invention
Aiming at the problem that present invention environmental pollution caused by existing undesirable the treatment effect of nickel and flyash, provide
A kind of preparation method and applications of the fly ash base adsorbent material of hydroxyl are administered in nickel contamination.
The present invention adopts the following technical scheme:
A kind of preparation method of the fly ash base adsorbent material of hydroxyl, includes the following steps:
The first step after mixing in proportion acrylic acid, diethanol amine and ethylene glycol, is added the concentrated sulfuric acid, is heated to reflux 3-6h,
Obtain mixed solution A；
Second step is proportionally added into acrylamide, after mixing, in 25 DEG C of items after neutralizing mixed solution A obtained by the first step
Under part, it is passed through nitrogen, is proportionally added into sodium hydrogensulfite and ammonium persulfate, at 20-40 DEG C, 5-10h is reacted, obtains mixing molten
Liquid B；
Third step is proportionally added into flyash into mixed solution B, under stirring condition, reacts 1-8h at 30-80 DEG C, is mixed
Close object；
4th step washes gained mixture, arrives hydroxyl fly ash base adsorbent material after drying.
In the first step, the mass ratio of the material of acrylic acid and diethanol amine is 1:0.1~1:1.1, acrylic acid and ethylene glycol
The mass ratio of the material is 1:0.1~1:1.1, and the mass ratio of the material of acrylic acid and the concentrated sulfuric acid is 1:0.8~1:2.
In second step, the mass ratio of the material of acrylamide and acrylic acid is 1:0.1~1:10, sodium hydrogensulfite and persulfuric acid
The mass ratio of the material of ammonium is 1:0.4~1:2, the amount summation and sodium hydrogensulfite and persulfuric acid of the substance of acrylamide and acrylic acid
The amount summation ratio of the substance of ammonium is 1:0.004~1:0.013.
In third step, the mass ratio of flyash and acrylic acid is 1:1.03~1:2.06.
A kind of fly ash base adsorbent material of hydroxyl is administered applied to nickel contamination.
Beneficial effects of the present invention are as follows:
1. flyash had not only been utilized with biggish surface area in the present invention, but its surface graft is some can be highly selective
Adsorb Ni2+Group, such as hydroxyl, amino, carboxyl, to improve its Ni2+Adsorptive selectivity, reduce nickel contamination the problem of.
2. flyash used in the present invention is a kind of solid waste, from a wealth of sources, flyash is both fully utilized,
The waste for realizing flyash is used again, and reduces environmental pollution.
3. Ni of the fly ash base adsorbent material for the hydroxyl that the present invention synthesizes in Adsorption water2+Aspect plays
Important function, the Ni that can be used in water removal2+, effectively solve the problems, such as that heavy metal nickel pollutes.
Detailed description of the invention
Fig. 1 is the principle of the present invention figure.
Specific embodiment
Embodiment 1
A kind of preparation method of the fly ash base adsorbent material of hydroxyl, including the following steps:
(1) after mixing by 1 mol acrylic acid, 0.5 mol diethanol amine and 0.5mol ethylene glycol, it is (dense that 2 mol sulfuric acid are added
Sulfuric acid), it is heated to reflux 3~6 h；
(2) after neutralizing acquired solution with NaOH solution, above-mentioned acquired solution is added in 1 mol acrylamide, is uniformly mixed,
It is passed through nitrogen at 25 DEG C, then is separately added at 20~40 DEG C of 0.007mol sodium hydrogensulfite and 0.006 mol ammonium persulfate and reacts 5
~10 h；
(3) 70 g flyash are added in above-mentioned solution, are stirred continuously, the reaction was continued at 30~80 DEG C 1~8 h；
(4) by the washing of gained mixture, drying, the fly ash base Ni of hydroxyl is obtained2+Adsorbent material is denoted as FMHNi-1.
The fly ash base adsorbent material of 50 mg hydroxyls is added to containing 50 mg/L Ni2+10 L water in, after 3 h
Respectively to Ni in water before and after the processing2+Content is detected, and the results are shown in Table 1.
Embodiment 2
The dosage of acrylic acid in 1 step of embodiment (1) is doubled, other steps are same as Example 1, gained adsorption material
Material, is denoted as FMHNi-2.
Remove Ni in water removal2+Experiment it is identical as embodiment 1, the results are shown in Table 1.
Embodiment 3
The dosage of diethanol amine in 1 step of embodiment (1) and the dosage of ethylene glycol are all doubled, other steps and embodiment
1 is identical, and gained adsorbent material is denoted as FMHNi-3.
Remove Ni in water removal2+Experiment it is identical as embodiment 1, the results are shown in Table 1.
Embodiment 4
Ammonium persulfate and sodium hydrogensulfite dosage in 1 step of embodiment (2) are doubled, other steps and 1 phase of embodiment
Together, gained adsorbent material is denoted as FMHNi-4.
Remove Ni in water removal2+Experiment it is identical as embodiment 1, the results are shown in Table 1.
Embodiment 5
Adsorbent material preparation step is same as Example 1.
The Ni in going water removal2+Experiment in, 100 mg fly ash base adsorbent material FMHCo-1 are added to containing 100
mg/L Ni2+10 L water in, respectively to Ni in water before and after the processing after 3 h2+Content is detected, and the results are shown in Table 1.
The adsorbent material of the present invention of table 1 and the prior art remove Ni2+Comparative result
As known from Table 1, the hydroxyl fly ash base adsorbent material prepared using preparation method of the invention is to the Ni in sewage2+
Adsorption rate is up to 99.9%, and can achieve document, (Hu Mingming, An Yan, Xu Meng fly the preparation of shaddock ped modified adsorbent and to Ni in water2+
Adsorption effect [J].Environmental science and technology, 2017,40 (6): 66-72) it is horizontal, but dosage is only the 1/75 of document, performance
Its excellent performance is gone out.And only to Ni2+There is efficient removal rate.
Claims (5)
1. a kind of preparation method of the fly ash base adsorbent material of hydroxyl, characterized by the following steps:
The first step after mixing in proportion acrylic acid, diethanol amine and ethylene glycol, is added the concentrated sulfuric acid, is heated to reflux 3-6h,
Obtain mixed solution A；
Second step is proportionally added into acrylamide, after mixing, in 25 DEG C of items after neutralizing mixed solution A obtained by the first step
Under part, it is passed through nitrogen, is proportionally added into sodium hydrogensulfite and ammonium persulfate, at 20-40 DEG C, 5-10h is reacted, obtains mixing molten
Liquid B；
Third step is proportionally added into flyash into mixed solution B, under stirring condition, reacts 1-8h at 30-80 DEG C, is mixed
Close object；
4th step washes gained mixture, arrives hydroxyl fly ash base adsorbent material after drying.
2. a kind of preparation method of the fly ash base adsorbent material of hydroxyl according to claim 1, it is characterised in that: the
In one step, the mass ratio of the material of acrylic acid and diethanol amine is 1:0.1~1:1.1, the mass ratio of the material of acrylic acid and ethylene glycol
For 1:0.1~1:1.1, the mass ratio of the material of acrylic acid and the concentrated sulfuric acid is 1:0.8~1:2.
3. a kind of preparation method of the fly ash base adsorbent material of hydroxyl according to claim 1, it is characterised in that: the
In two steps, the mass ratio of the material of acrylamide and acrylic acid is 1:0.1~1:10, the substance of sodium hydrogensulfite and ammonium persulfate
Amount than being 1:0.4~1:2, the substance of the amount summation and sodium hydrogensulfite and ammonium persulfate of the substance of acrylamide and acrylic acid
Amount summation ratio is 1:0.004~1:0.013.
4. a kind of preparation method of the fly ash base adsorbent material of hydroxyl according to claim 1, it is characterised in that: the
In three steps, the mass ratio of flyash and acrylic acid is 1:1.03~1:2.06.
5. a kind of fly ash base adsorbent material of the hydroxyl as described in Claims 1-4 any one is controlled applied to nickel contamination
Reason.
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|---|---|---|---|
| CN201811068994.5A CN109126723B (en) | 2018-09-13 | 2018-09-13 | Preparation method of fly ash-based adsorption material containing hydroxyl and application of fly ash-based adsorption material in nickel pollution treatment |
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| CN201811068994.5A CN109126723B (en) | 2018-09-13 | 2018-09-13 | Preparation method of fly ash-based adsorption material containing hydroxyl and application of fly ash-based adsorption material in nickel pollution treatment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232539A (en) * | 2022-09-05 | 2022-10-25 | 华电电力科学研究院有限公司 | Wear-resistant UV (ultraviolet) coating and preparation method thereof |
| CN116510744A (en) * | 2023-04-26 | 2023-08-01 | 浙江天地环保科技股份有限公司 | Preparation of nickel-manganese modified fly ash ozone oxidation catalyst by hot alkali method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232539A (en) * | 2022-09-05 | 2022-10-25 | 华电电力科学研究院有限公司 | Wear-resistant UV (ultraviolet) coating and preparation method thereof |
| CN116510744A (en) * | 2023-04-26 | 2023-08-01 | 浙江天地环保科技股份有限公司 | Preparation of nickel-manganese modified fly ash ozone oxidation catalyst by hot alkali method |
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| CN109126723B (en) | 2021-04-16 |
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