CN109126647A - A kind of preparation method of graphene oxide-sodium alginate gel ball - Google Patents
A kind of preparation method of graphene oxide-sodium alginate gel ball Download PDFInfo
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- CN109126647A CN109126647A CN201811046804.XA CN201811046804A CN109126647A CN 109126647 A CN109126647 A CN 109126647A CN 201811046804 A CN201811046804 A CN 201811046804A CN 109126647 A CN109126647 A CN 109126647A
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- graphene oxide
- coal slime
- deionized water
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- gel ball
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0065—Preparation of gels containing an organic phase
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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
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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
-
- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
-
- 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
Abstract
The present invention relates to a kind of graphene oxide-sodium alginate gel ball preparation methods, belong to environmental friendly material technical field.The present invention is modified coal slime, so that particle surface becomes coarse, increase specific surface area, enhance adsorption capacity, simultaneously by modified, the hydrogen ion of particle surface hydroxyl can dissociate, so that the elecrtonegativity of particle surface enhances, can adsorb positively charged metal ion or cationic pollutant；In surface of graphene oxide carried titanium dioxide, enable gel ball that pollutant is decomposed into water and carbon dioxide in the sun or under ultraviolet light, degrades while adsorbing pollutant to it, improve the treatment effeciency to pollutant；The gel ball that the present invention is formed using sodium alginate is matrix, surface mixes modified coal slime particle, gel ball is coated with the graphene oxide for having loaded nano-titanium dioxide, gel ball quick adsorption is polluted and carries out photocatalytic degradation, adsorption time is short, adsorption capacity is strong.
Description
Technical field
The present invention relates to a kind of graphene oxide-sodium alginate gel ball preparation methods, belong to environmental friendly material technology
Field.
Background technique
Water body is is one of the main natural resources on which mankind depends, and is an important part of the human ecological environment,
It is also the storage cavern of substance biogeochemical cycle, there is certain sensibility to environment.Due to the influence of mankind's activity, enter
Polluter in water body environment is more and more, these pollutants cause many problems to environmental and human health impacts.Especially
With the development of the industries such as mining, smelting, chemical industry, plating, electronics, process hides and civilian solid waste it is unreasonable landfill and
It stacks, the application of heavy metal contaminants accidental release and a large amount of chemical fertilizer, pesticide, so that various heavy metal contaminants enter water
Body.Heavy metal contaminants are difficult to administer, they have quite high stability and refractory organics in water body.Heavy metal is in water body
In run up to certain limit and will generate serious harm to water body-water plant-aquatic animal system, and food may be passed through
Chain directly or indirectly influences the own health of the mankind.It can be said that heavy metal pollution of water body has become in the world today
One of environmental problem of most serious, and how scientificlly and effectively to solve heavy metal and countries in the world political affairs are had become to the pollution of water body
One of the hot spot of mansion and numerous environmental workers research.
The research of repairing and treating heavy metal pollution of water body is that most commonly used research contents is carried out in countries in the world, almost each
A country all suffers from different degrees of heavy metal pollution of water body problem, so the research of this respect is concerned.Generally speaking,
Heavy metal pollution of water body repairing and treating uses following two Basic Ways, first is that reduce transfer ability of the heavy metal in water body and
Bioavailability；
Second is that heavy metal is thoroughly removed from contaminated water body.More common chemical coagulation, absorption method and electricity are repaired below
Multiple method is briefly introduced: chemical coagulation, absorption method: many heavy metals mainly exist in water body solution with cation, increase
Water pH value can make most of heavy metals generate hydroxide precipitating.In addition, other numerous anion can also make accordingly
Heavy metal ion forms precipitating.Accordingly, apply the substances such as lime, calcium carbonate to contaminated by heavy metals water body, can reduce weight
The extent of injury of the metal to water body.
Electric repairing method is the heavy metal pollution of water body recovery technique that the 1990s, Later development got up.Its basic principle
It is to the water body both ends by heavy metal pollution plus DC electric field, using electric field migration force by heavy metal transformation water-outlet body.
In recent years, sodium alginate is often applied to the embedding medium of immobilized cell, but its gel in terms of heavy metal improvement
There are still adsorption time length, the problem of adsorption capacity deficiency for ball, it is difficult to meet answering for paroxysmal para-aminophenol contamination accident
Anxious quickly disposition requires.And it is more rare as the research in terms of heavy metal absorbent in graphene oxide-sodium alginate.
Summary of the invention
The technical problems to be solved by the invention: for gel ball now, there are adsorption time length, adsorption capacity deficiency, hardly possible
The problem of requiring quickly is disposed to meet the emergency of abrupt polluting accident, it is solidifying to propose a kind of graphene oxide-sodium alginate
The preparation method of glueballs.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) it takes coal slime and rinses it with deionized water, grind, sieve with 100 mesh sieve after drying, obtain dry coal slime；
(2) dry coal slime is put into the sodium hydroxide solution of 2mol/L, heating stirring is carried out under the conditions of 50 DEG C, be uniformly mixed,
Coal slime is filtered out afterwards for 24 hours, and is rinsed 5 ~ 8 times with 60 DEG C of deionized water, baking oven drying is subsequently placed in, obtains alkalization coal slime；
(3) it takes alkalization coal slime, cetyl trimethylammonium bromide and deionized water to be uniformly mixed, stirs for 24 hours, obtain under the conditions of 25 DEG C
To mixed liquor；
(4) mixed liquor is filtered, filter residue is cleaned 5 ~ 8 times with 100g30 DEG C of deionized water, crosses 200 mesh after then grinding
Sieve obtains modified coal slime；
(5) butyl titanate, dehydrated alcohol, ammonium chloride and deionized water are taken, is uniformly mixed and obtains solution A；
(6) graphene oxide and deionized water is taken to mix, ultrasonic 2h obtains dispersion liquid, be added in dispersion liquid glucose and
13mol/L ammonia spirit stirs 10min, obtains solution B；
(7) solution A and solution B are mixed, reacts 4h under the conditions of 160 DEG C of glycerol baths, obtains reaction solution, reaction solution is filtered, it will
Filter residue drying, obtains modified graphene oxide；
(8) modified coal slime, lauryl sodium sulfate, modified graphene oxide, sodium alginate and deionized water mixing, stirring are taken
10min obtains suspension；
(9) suspension is instilled in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel ball is obtained after solidification.
The mass ratio of step (1) coal slime and deionized water is 1:10.
The mass ratio of step (2) the dry coal slime, sodium hydroxide solution and deionized water is 1:5:10.
The mass ratio of step (3) the alkalization coal slime, cetyl trimethylammonium bromide and deionized water is 4:1:20.
Step (5) butyl titanate, dehydrated alcohol, ammonium chloride and deionized water mass ratio be 1:20:20:25.
Step (6) graphene oxide, deionized water, glucose and ammonium hydroxide mass ratio be 1:50:1:5.
Step (8) the modified coal slime, lauryl sodium sulfate, modified graphene oxide, sodium alginate and deionized water
Mass ratio be 3:1:1:50.
The present invention is compared with other methods, and advantageous effects are:
(1) coal slime is the waste material that coal yard generates, abundance and cheap, after being modified to it, is enabled to
Grain surface becomes coarse, increases specific surface area, enhances adsorption capacity, while passing through modified, the hydrogen of particle surface hydroxyl
Ion can dissociate so that the elecrtonegativity of particle surface enhances, can adsorb positively charged metal ion or sun from
Sub- pollutant；
(2) there are graphene oxide many superior properties after its area load titanium dioxide gel ball is existed
It is decomposed into water and carbon dioxide under sunlight or by pollutant under ultraviolet light, it is dropped while adsorbing pollutant
Solution, substantially increases the treatment effeciency to pollutant；
(3) gel ball that graphene oxide-sodium alginate gel ball prepared by the present invention is formed using sodium alginate is matrix, table
Face mixes modified coal slime particle, is finally coated with the graphene oxide for having loaded nano-titanium dioxide to gel ball, so that
Gel ball can quick adsorption pollute and carry out photocatalytic degradation, solve ordinary gel ball adsorption time is long, adsorption capacity not
Strong disadvantage.
Specific embodiment
It takes 10 ~ 20g coal slime and rinses it with 100 ~ 200g deionized water, grind, sieve with 100 mesh sieve after drying, done
Dry coal slime；The dry coal slime of 5 ~ 10g is put into the sodium hydroxide solution of 25 ~ 50g2mol/L, heating is carried out under the conditions of 50 DEG C and is stirred
It mixes, is uniformly mixed, for 24 hours afterwards filters out coal slime, and rinsed 5 ~ 8 times with 50 ~ 100g60 DEG C of deionized water, be subsequently placed in baking oven baking
It is dry, obtain alkalization coal slime；Take 4 ~ 8g alkalization coal slime, 1 ~ 2g cetyl trimethylammonium bromide and the mixing of 20 ~ 40g deionized water equal
It is even, it is stirred under the conditions of 25 DEG C for 24 hours, obtains mixed liquor；Mixed liquor is filtered, filter residue is cleaned with 100g30 DEG C of deionized water
5 ~ 8 times, 200 meshes are crossed after then grinding, obtain modified coal slime；Take 2 ~ 4g butyl titanate, 40 ~ 80g dehydrated alcohol, 40 ~ 80g chlorine
Change ammonium and 50 ~ 100g deionized water, is uniformly mixed and obtains solution A；Take 1 ~ 2g graphene oxide and 50 ~ 100g deionized water mixed
It closes, ultrasonic 2h obtains dispersion liquid, and 1 ~ 2g glucose and 5 ~ 10g13mol/L ammonia spirit, stirring are added in dispersion liquid
10min obtains solution B；Solution A and solution B are mixed, 4h is reacted under the conditions of 160 DEG C of glycerol baths, obtains reaction solution, will react
Liquid filters, and filter residue is dried, modified graphene oxide is obtained；The modified coal slime of 3 ~ 5g, 1 ~ 2g lauryl sodium sulfate, 1 ~ 2g is taken to change
Property graphene oxide, 5 ~ 10g sodium alginate and 50 ~ 100g deionized water mixing, stir 10min, obtain suspension；By suspension
It instills in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel ball is obtained after solidification.
It takes 10g coal slime and rinses it with 100g deionized water, grind, sieve with 100 mesh sieve after drying, obtain dry coal slime；
The dry coal slime of 5g is put into the sodium hydroxide solution of 25g2mol/L, heating stirring is carried out under the conditions of 50 DEG C, is uniformly mixed, for 24 hours
Coal slime is filtered out afterwards, and is rinsed 5 times with 50g60 DEG C of deionized water, baking oven drying is subsequently placed in, obtains alkalization coal slime；Take 4g
Coal slime, 1g cetyl trimethylammonium bromide and the 20g deionized water of alkalizing are uniformly mixed, and are stirred for 24 hours, are mixed under the conditions of 25 DEG C
Close liquid；Mixed liquor is filtered, filter residue is cleaned 5 times with 100g30 DEG C of deionized water, 200 meshes is crossed after then grinding, obtains
To modified coal slime；2g butyl titanate, 40g dehydrated alcohol, 40g ammonium chloride and 50g deionized water are taken, is uniformly mixed and obtains solution A；
Take 1g graphene oxide and 50g deionized water to mix, ultrasonic 2h obtains dispersion liquid, be added in dispersion liquid 1g glucose and
5g13mol/L ammonia spirit stirs 10min, obtains solution B；Solution A and solution B are mixed, it is anti-under the conditions of 160 DEG C of glycerol baths
4h is answered, reaction solution is obtained, reaction solution is filtered, filter residue is dried, obtains modified graphene oxide；Take 3g modified coal slime, 1g ten
Sodium dialkyl sulfate, 1g modified graphene oxide, 5g sodium alginate and the mixing of 50g deionized water, stir 10min, are suspended
Liquid；Suspension is instilled in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel ball is obtained after solidification.
It takes 15g coal slime and rinses it with 150g deionized water, grind, sieve with 100 mesh sieve after drying, obtain dry coal slime；
The dry coal slime of 7g is put into the sodium hydroxide solution of 37g2mol/L, heating stirring is carried out under the conditions of 50 DEG C, is uniformly mixed, for 24 hours
Coal slime is filtered out afterwards, and is rinsed 7 times with 75g60 DEG C of deionized water, baking oven drying is subsequently placed in, obtains alkalization coal slime；Take 6g
Coal slime, 1.5g cetyl trimethylammonium bromide and the 30g deionized water of alkalizing are uniformly mixed, and are stirred for 24 hours, are obtained under the conditions of 25 DEG C
Mixed liquor；Mixed liquor is filtered, filter residue is cleaned 7 times with 100g30 DEG C of deionized water, crosses 200 meshes after then grinding,
Obtain modified coal slime；3g butyl titanate, 60g dehydrated alcohol, 60g ammonium chloride and 75g deionized water are taken, is uniformly mixed and obtains solution
A；1.5g graphene oxide and 75g deionized water is taken to mix, ultrasonic 2h obtains dispersion liquid, and 1.5g grape is added in dispersion liquid
Sugar and 7g13mol/L ammonia spirit stir 10min, obtain solution B；Solution A and solution B are mixed, 160 DEG C of glycerol bath conditions
Lower reaction 4h, obtains reaction solution, reaction solution is filtered, filter residue is dried, obtain modified graphene oxide；Take the modified coal slime of 4g,
1.5g lauryl sodium sulfate, 1.5g modified graphene oxide, 7g sodium alginate and the mixing of 75g deionized water, stir 10min,
Obtain suspension；Suspension is instilled in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel is obtained after solidification
Ball.
It takes 20g coal slime and rinses it with 200g deionized water, grind, sieve with 100 mesh sieve after drying, obtain dry coal slime；
The dry coal slime of 10g is put into the sodium hydroxide solution of 50g2mol/L, heating stirring is carried out under the conditions of 50 DEG C, is uniformly mixed,
Coal slime is filtered out afterwards for 24 hours, and is rinsed 8 times with 100g60 DEG C of deionized water, baking oven drying is subsequently placed in, obtains alkalization coal slime；
It takes 8g alkalization coal slime, 2g cetyl trimethylammonium bromide and 40g deionized water to be uniformly mixed, stirs for 24 hours, obtain under the conditions of 25 DEG C
To mixed liquor；Mixed liquor is filtered, filter residue is cleaned 8 times with 100g30 DEG C of deionized water, crosses 200 mesh after then grinding
Sieve obtains modified coal slime；4g butyl titanate, 80g dehydrated alcohol, 80g ammonium chloride and 100g deionized water are taken, is uniformly mixed and obtains
Solution A；2g graphene oxide and 100g deionized water is taken to mix, ultrasonic 2h obtains dispersion liquid, and 2g grape is added in dispersion liquid
Sugar and 10g13mol/L ammonia spirit stir 10min, obtain solution B；Solution A and solution B are mixed, 160 DEG C of glycerol bath conditions
Lower reaction 4h, obtains reaction solution, reaction solution is filtered, filter residue is dried, obtain modified graphene oxide；Take the modified coal slime of 5g,
2g lauryl sodium sulfate, 2g modified graphene oxide, 10g sodium alginate and the mixing of 100g deionized water, stir 10min, obtain
To suspension；Suspension is instilled in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel is obtained after solidification
Ball.
Graphene oxide prepared by the present invention-sodium alginate gel ball and commercially available gel ball are detected, it is specific to detect
As a result such as following table table 1:
Detection method: take that 0.25g graphene oxide-sodium alginate gel ball is added to 50mL lead ion, concentration of cadmium ions is all
In the water of 10mg/L, oscillation absorption 1.5h is carried out on HY-4 speed regulation multi-purpose type oscillator, uses inductivity coupled plasma mass spectrometry
Instrument (ICP) detects Heavy Metals in Waters content.
1 graphene oxide of table-sodium alginate gel ball performance characterization
Graphene oxide prepared by the present invention-sodium alginate gel ball as shown in Table 1, in a short time to the metal ion in water
Adsorption efficiency it is high, have a extensive future.
Claims (7)
1. a kind of graphene oxide-sodium alginate gel ball preparation method, which is characterized in that specific production step is
(1) it takes coal slime and rinses it with deionized water, grind, sieve with 100 mesh sieve after drying, obtain dry coal slime；
(2) dry coal slime is put into the sodium hydroxide solution of 2mol/L, heating stirring is carried out under the conditions of 50 DEG C, be uniformly mixed,
Coal slime is filtered out afterwards for 24 hours, and is rinsed 5 ~ 8 times with 60 DEG C of deionized water, baking oven drying is subsequently placed in, obtains alkalization coal slime；
(3) it takes alkalization coal slime, cetyl trimethylammonium bromide and deionized water to be uniformly mixed, stirs for 24 hours, obtain under the conditions of 25 DEG C
To mixed liquor；
(4) mixed liquor is filtered, filter residue is cleaned 5 ~ 8 times with 100g30 DEG C of deionized water, crosses 200 mesh after then grinding
Sieve obtains modified coal slime；
(5) butyl titanate, dehydrated alcohol, ammonium chloride and deionized water are taken, is uniformly mixed and obtains solution A；
(6) graphene oxide and deionized water is taken to mix, ultrasonic 2h obtains dispersion liquid, be added in dispersion liquid glucose and
13mol/L ammonia spirit stirs 10min, obtains solution B；
(7) solution A and solution B are mixed, reacts 4h under the conditions of 160 DEG C of glycerol baths, obtains reaction solution, reaction solution is filtered, it will
Filter residue drying, obtains modified graphene oxide；
(8) modified coal slime, lauryl sodium sulfate, modified graphene oxide, sodium alginate and deionized water mixing, stirring are taken
10min obtains suspension；
(9) suspension is instilled in 500g saturation calcium chloride solution, graphene oxide-sodium alginate gel ball is obtained after solidification.
2. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (1) described coal slime and deionized water is 1:10.
3. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (2) described dry coal slime, sodium hydroxide solution and deionized water is 1:5:10.
4. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (3) described alkalization coal slime, cetyl trimethylammonium bromide and deionized water is 4:1:20.
5. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (5) described butyl titanate, dehydrated alcohol, ammonium chloride and deionized water is 1:20:20:25.
6. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (6) described graphene oxide, deionized water, glucose and ammonium hydroxide is 1:50:1:5.
7. a kind of preparation method of graphene oxide-sodium alginate gel ball as described in claim 1, which is characterized in that step
Suddenly the mass ratio of (8) described modified coal slime, lauryl sodium sulfate, modified graphene oxide, sodium alginate and deionized water is
3:1:1:50。
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| CN109939705A (en) * | 2019-04-15 | 2019-06-28 | 福建农林大学 | A kind of multi-element biologic matter aerogel composite and preparation method thereof for photocatalytic reduction of carbon oxide |
| CN111001393A (en) * | 2019-12-24 | 2020-04-14 | 北方工业大学 | Sodium alginate-based loaded nano-red titanium manganese ore/brown coal-based active coke hydrogel and preparation method thereof |
| CN114950498A (en) * | 2022-05-16 | 2022-08-30 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
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| CN114950498A (en) * | 2022-05-16 | 2022-08-30 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
| CN114950498B (en) * | 2022-05-16 | 2023-12-22 | 江苏农林职业技术学院 | Recyclable efficient photocatalytic material and preparation method and application thereof |
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