CN106902791A - A kind of modified attapulgite earth adsorbing and preparation method - Google Patents
A kind of modified attapulgite earth adsorbing and preparation method Download PDFInfo
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Abstract
The invention discloses a kind of modified attapulgite earth adsorbing and preparation method, belong to technical field of absorbent.The adsorbent includes following component：Modified attapulgite clay, polyacrylamide modified graphene and appropriate solvent.Preparation method includes：Concave-convex clay rod pretreatment is first removed into mud and impurity, then by hydrochloric Acid Modification, finally the modified Concave-convex clay rod of acid and polyacrylamide modified graphene are added in conical flask, add water, stir, then 30 ~ 50min of ultrasound, vacuum filtration, drying in vacuum drying chamber is subsequently placed in, particle diameter is ground to for 100 ~ 200 mesh, the modified attapulgite adsorbent is obtained final product.The adsorbent has preferable adsorption and sedimentation efficiency, can effectively remove heavy metal ion and coloring matter in waste water, for the safety dumping of waste water provides guarantee, with preferable application value.And preparation method is simple, mild condition, time-consuming short, is adapted to industrial production.
Description
Technical field
The present invention relates to technical field of absorbent, and in particular to a kind of modified attapulgite earth adsorbing and preparation method.
Background technology
Effluent containing heavy metal ions are one of big water environment pollution modes in the world today three, and these effluent containing heavy metal ions enter
Can not be biodegradable after environment, certain limit is run up in water body will produce to water body-water plant-aquatic animal system
Raw serious harm, and the health of mankind itself can be had influence on by food chain.Existing heavy metal processing method mainly includes changing
Learn the methods, wherein chemical precipitation method application such as precipitation, solvent extraction, ion exchange, UF membrane, activated carbon and silica gel absorption the most
Extensively, but for low concentration wastewater, using chemical precipitation method, in the presence of investing, big, operating cost is high and is also easy to produce secondary pollution
Problem.And absorption method because its material is cheap and easily-available, low cost and removal effect it is good turn into research emphasis, it is most normal at present both at home and abroad
Adsorbent is activated carbon, but activated carbon has that high cost, absorption are easily saturated and regenerate difficulty, therefore seek
The substitute products of activated carbon are looked for be paid close attention to by this area.
Attapulgite, with special fibre structure and crystal structure, is allowed to many spies as a kind of natural material
Different materialization and processing performance, the good reputation for having " kings of thousand soil " and " soil of general-purpose ".Because attapulgite has larger ratio table
Area, makes it have stronger suction-operated, therefore attapulgite is applied into wastewater treatment and closed by more more and more people
Note.
The Chinese invention patent of Application No. 201410288153.0 disclose a kind of granular concave rod earth adsorbing and its
Preparation method.Its technical scheme is：Water is well mixed with attapulgite powder, the mass ratio 1 of water and attapulgite powder：
0.5~1, pureed attapulgite is obtained；Obtained pureed attapulgite is dried into 8~16h under the conditions of 90~110 DEG C again, is broken
It is broken to the granular concave rod soil that particle diameter is 0.45~1.25mm；Then obtained granular concave rod soil is placed in Muffle furnace,
2~3h is calcined under the conditions of 650~750 DEG C, granular concave rod earth adsorbing is obtained.Although methods described does not produce secondary pollution,
The characteristics of prepared granular concave rod earth adsorbing has big particle diameter, free settling, easily recovery and absorption property are good, but institute
Time-consuming, condition harsh to state preparation technology, with cost of manufacture higher, is not suitable for popularization and application.
Therefore, researching and developing one kind both has preferable adsorption and sedimentation effect, and with the gentle concave convex rod of reaction condition
Earth adsorbing turns into the emphasis of research at present, it may have preferable application prospect and use value.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of modified attapulgite earth adsorbing and preparation side
Method, the modified attapulgite earth adsorbing has preferably dispersiveness and adsorption and sedimentation efficiency, in can effectively removing waste water
Heavy metal ion and coloring matter, for the safety dumping of waste water provides guarantee, with preferable application value.Additionally, described
Preparation method is simple, mild condition, time-consuming short, suitable industrial production.
The present invention solves technical problem and adopts the following technical scheme that：
The present invention relates to a kind of modified attapulgite earth adsorbing, including following parts by weight each component：Modified attapulgite glues
Native 20 ~ 40 parts, 10 ~ 20 parts of polyacrylamide modified graphene, also including appropriate solvent.
Preferably, the modified attapulgite clay is the modified Concave-convex clay rod of acid.
Preferably, the solvent includes first alcohol and water.
The invention further relates to a kind of method for preparing modified attapulgite earth adsorbing, comprise the following steps：
（1）The pretreatment of Concave-convex clay rod：Natural attapulgite clay is carried out to be crushed to 100 ~ 200 mesh, is added water, stir shape
Into mud in suspension, then by ultrasound it is fully dispersed after, take upper suspension in the centrifuge of 3000 turns/min centrifugal treating 5 ~
10min, vacuum filtration obtains Concave-convex clay rod one after standing；
Concave-convex clay rod one is placed in beaker, methyl alcohol is added, in 10 ~ 20min of ultrasound, vacuum after standing under Ultrasonic Conditions
Suction filtration, is dried to obtain Concave-convex clay rod two；
（2）The preparation of modified attapulgite clay：Concave-convex clay rod two is placed in flask, the watery hydrochloric acid of 2mol/L is added,
In 10 ~ 20min of ultrasound, vacuum filtration under Ultrasonic Conditions, and cleaned with distilled water, then dried in vacuum drying chamber, ground
100 ~ 200 mesh are milled to, modified Concave-convex clay rod is obtained final product；
（3）The preparation of polyacrylamide modified graphene：10 ~ 20 parts of graphene oxide is weighed, 10 ~ 20 times of graphene oxide is added
The water of weight, through 20 ~ 30min of ultrasonication, adds acrylamide monomer, ammonium persulfate, is stirred under the conditions of 80 DEG C ~ 90 DEG C
3 ~ 5h of reaction is mixed, purification obtains the modified graphene oxide of polyacrylamide；
To distilled water is added in modified graphene oxide, adding vitamin C carries out 2 ~ 3h of reduction reaction, vacuum filtration,
And wash, obtain final product polyacrylamide modified graphene；
（4）Modified attapulgite adsorbent：According to proportioning by modified Concave-convex clay rod and polyacrylamide modified graphite
Alkene is added in conical flask, is added water, and is stirred, and is subsequently placed in 30 ~ 50min of ultrasound under Ultrasonic Conditions, vacuum filtration, then
It is placed in vacuum drying chamber and dries, be ground to particle diameter for 100 ~ 200 mesh, obtains final product the modified attapulgite adsorbent.
Preferably, the step（1）In the weight that adds water be 3 ~ 8 times of Concave-convex clay rod weight.
Preferably, the step（1）The addition volume of middle methyl alcohol is 50mL with Concave-convex clay rod mass ratio：5~10g.
Preferably, the step（2）The addition volume of middle watery hydrochloric acid：Concave convex rod quality is 1mL：2g~5g.
Preferably, the step（2）In distillation water cleaning method include：Concave-convex clay rod after suction filtration is added and is burnt
In cup, distilled water is added, be placed in ultrasound 5min under Ultrasonic Conditions, be repeated 2 times operation.
Preferably, the step（3）The acrylamide monomer of middle addition is 0.1 ~ 1 part, and its quality is ammonium persulfate quality
10 ~ 20 times.
The reason for from this scope is：Graphene can greatly improve its hanging in water in the modified lower of polyacrylamide
Floating amount, with increasing for acrylamide addition, the suspension amount of modified graphene dispersion in water can also increase, but work as
The addition of acrylamide to Graphene consumption more than 0.1 when, can cause that the content of polyacrylamide is much, product viscosity increase
Height, ultimately results in suspension amount of the Graphene in water and substantially reduces.
Preferably, the step（3）Middle washing process is first washed with distillation, and again with methanol is washed, then is washed with distillation.
Compared with prior art, the present invention has following beneficial effect：
（1）The modified attapulgite earth adsorbing that the present invention is prepared, with preferable adsorption and sedimentation efficiency, can effectively remove
Heavy metal ion and coloring matter in waste water, for the safety dumping of waste water provides guarantee, it is to avoid because wastewater treatment does not reach
Environmental pollution caused by mark, while the cost of wastewater treatment is reduced, with preferable application value.Additionally, the preparation side
Method is simple, mild condition, time-consuming short, suitable industrial production.
（2）It is absorption carrier that the present invention uses Concave-convex clay rod, because Concave-convex clay rod has larger specific surface
Product, makes it have preferable adsorption bleaching characteristic；Due to attapulgite rich reserves, cost of manufacture is cheap；Along with concave convex rod
Penus natural nano-material, environmental protection will not cause secondary pollution to environment, meet the requirement of environmentally friendly product, tool
There is preferable use value.
（3）The present invention uses polyacrylamide modified graphene as the modifying agent of Concave-convex clay rod, due to polypropylene
The structure of the Graphene of amide modifications is the surface grafting polyacrylamide segment in Graphene so that Graphene has in water
Preferably, more uniform dispersion effect, and then cause that modified attapulgite also inherits this advantage so that modified is concavo-convex
Rod soil is more uniformly dispersed in waste water, the utilization rate and adsorption bleaching ability of attapulgite is considerably increased, so as to be fast
Fast efficient wastewater treatment is provided and ensured.
（4）The characteristics of modified attapulgite earth adsorbing that the present invention is prepared also has repeatable utilization, substantially reduces
The use cost of adsorbent, improves raw material availability, is adapted to industrialization promotion, with preferable Practical significance.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.
Embodiment 1：
A kind of modified attapulgite earth adsorbing and preparation method of the preferred embodiment of the present invention；
The modified attapulgite earth adsorbing is prepared from by each component of following parts by weight：Modified attapulgite clay 40
Part, 15 parts of polyacrylamide modified graphene, also including appropriate solvent.Wherein, modified attapulgite clay is sour modified
Concave-convex clay rod, solvent include first alcohol and water.
The preparation method of the modified attapulgite earth adsorbing, comprises the following steps：
（1）The pretreatment of Concave-convex clay rod：Natural attapulgite clay is carried out to be crushed to 200 mesh, adds attapulgite to glue
5 times of the native weight water of amount, stirring forms mud in suspension, then by ultrasound it is fully dispersed after, take upper suspension in 3000 turns/
The min of centrifugal treating 8 in the centrifuge of min, vacuum filtration obtains Concave-convex clay rod one after standing；
Concave-convex clay rod one is placed in beaker, methyl alcohol is added, in ultrasonic 15 min under Ultrasonic Conditions, vacuum is taken out after standing
Filter, is dried to obtain Concave-convex clay rod two, wherein, addition volume and the Concave-convex clay rod mass ratio of methyl alcohol are 50mL：8 g；
（2）The preparation of modified attapulgite clay：Concave-convex clay rod two is placed in flask, the watery hydrochloric acid of 2mol/L is added,
In ultrasonic 15 min, vacuum filtration under Ultrasonic Conditions, and cleaned with distilled water, then dried in vacuum drying chamber, grinding
To 200 mesh, modified Concave-convex clay rod is obtained final product, wherein, the addition volume of watery hydrochloric acid：Concave convex rod quality is 1mL：3g；
（3）The preparation of polyacrylamide modified graphene：15 parts of graphene oxide is weighed, 15 times of weight of graphene oxide are added
Water, through the min of ultrasonication 20, adds acrylamide monomer, ammonium persulfate, and the h of stirring reaction 5, carries under the conditions of 80 DEG C
It is pure to obtain the modified graphene oxide of polyacrylamide；
To distilled water is added in modified graphene oxide, adding vitamin C carries out the h of reduction reaction 2, vacuum filtration, and
Washing, obtains final product polyacrylamide modified graphene；
（4）Modified attapulgite adsorbent：According to proportioning by modified Concave-convex clay rod and polyacrylamide modified graphite
Alkene is added in conical flask, is added water, and is stirred, and is subsequently placed in ultrasonic 40 min under Ultrasonic Conditions, and then vacuum filtration is put
Dried in vacuum drying chamber, be ground to particle diameter for 200 mesh, obtain final product the modified attapulgite adsorbent.
Step（2）In distillation water cleaning method include：By in the Concave-convex clay rod addition beaker after suction filtration, add and steam
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（3）The acrylamide monomer of middle addition is 0.5 part, and its quality is 15 times of ammonium persulfate quality.
Step（3）Middle washing process is first washed with distillation, and again with methanol is washed, then is washed with distillation, can fully be washed
Adsorb the acrylamide and polyacrylamide and other impurities in graphenic surface.
Embodiment 2：
A kind of modified attapulgite earth adsorbing and preparation method of the preferred embodiment of the present invention；
Modified attapulgite earth adsorbing, is prepared from by each component of following parts by weight：It is 30 parts of modified attapulgite clay, poly-
10 parts of acrylic amide modified Graphene, also including appropriate solvent.Wherein, modified attapulgite clay is modified concavo-convex acid
Rod stone clay, solvent includes first alcohol and water.
The preparation method of modified attapulgite earth adsorbing, comprises the following steps：
（1）The pretreatment of Concave-convex clay rod：Natural attapulgite clay is carried out to be crushed to 100 mesh, adds attapulgite to glue
3 times of the native weight water of amount, stirring forms mud in suspension, then by ultrasound it is fully dispersed after, take upper suspension in 3000 turns/
The min of centrifugal treating 5 in the centrifuge of min, vacuum filtration obtains Concave-convex clay rod one after standing；
Concave-convex clay rod one is placed in beaker, methyl alcohol is added, in ultrasonic 20 min under Ultrasonic Conditions, vacuum is taken out after standing
Filter, is dried to obtain Concave-convex clay rod two, wherein, addition volume and the Concave-convex clay rod mass ratio of methyl alcohol are 50mL：5g；
（2）The preparation of modified attapulgite clay：Concave-convex clay rod two is placed in flask, the watery hydrochloric acid of 2mol/L is added,
In ultrasonic 10 min, vacuum filtration under Ultrasonic Conditions, and cleaned with distilled water, then dried in vacuum drying chamber, grinding
To 100 mesh, modified Concave-convex clay rod is obtained final product, wherein, the addition volume of watery hydrochloric acid：Concave convex rod quality is 1mL：2g；
（3）The preparation of polyacrylamide modified graphene：10 parts of graphene oxide is weighed, 10 times of weight of graphene oxide are added
Water, through the min of ultrasonication 20, adds acrylamide monomer, ammonium persulfate, and the h of stirring reaction 3, carries under the conditions of 90 DEG C
It is pure to obtain the modified graphene oxide of polyacrylamide；
To distilled water is added in modified graphene oxide, adding vitamin C carries out reduction reaction 2h, vacuum filtration, and
Washing, obtains final product polyacrylamide modified graphene；
（4）Modified attapulgite adsorbent：According to proportioning by modified Concave-convex clay rod and polyacrylamide modified graphite
Alkene is added in conical flask, is added water, and is stirred, and is subsequently placed in ultrasonic 30 min under Ultrasonic Conditions, and then vacuum filtration is put
Dried in vacuum drying chamber, be ground to particle diameter for 100 mesh, obtain final product the modified attapulgite adsorbent.
Step（2）In distillation water cleaning method include：By in the Concave-convex clay rod addition beaker after suction filtration, add and steam
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（3）The acrylamide monomer of middle addition is 0.1 part, and its quality is 10 times of ammonium persulfate quality.
Step（3）Middle washing process is first washed with distillation, and again with methanol is washed, then is washed with distillation, can fully be washed
Adsorb the acrylamide and polyacrylamide and other impurities in graphenic surface.
Embodiment 3：
A kind of modified attapulgite earth adsorbing and preparation method of the preferred embodiment of the present invention；
Modified attapulgite earth adsorbing, is prepared from by each component of following parts by weight：It is 50 parts of modified attapulgite clay, poly-
20 parts of acrylic amide modified Graphene, also including appropriate solvent.Wherein, modified attapulgite clay is modified concavo-convex acid
Rod stone clay, solvent includes first alcohol and water.
The preparation method of modified attapulgite earth adsorbing, comprises the following steps：
（1）The pretreatment of Concave-convex clay rod：Natural attapulgite clay is carried out to be crushed to 200 mesh, adds attapulgite to glue
8 times of the native weight water of amount, stirring forms mud in suspension, then by ultrasound it is fully dispersed after, take upper suspension in 3000 turns/
Centrifugal treating 10min in the centrifuge of min, vacuum filtration obtains Concave-convex clay rod one after standing；
Concave-convex clay rod one is placed in beaker, methyl alcohol is added, in ultrasonic 10 min under Ultrasonic Conditions, vacuum is taken out after standing
Filter, is dried to obtain Concave-convex clay rod two, wherein, addition volume and the Concave-convex clay rod mass ratio of methyl alcohol are 50mL：10g；
（2）The preparation of modified attapulgite clay：Concave-convex clay rod two is placed in flask, the watery hydrochloric acid of 2mol/L is added,
In ultrasound 20min, vacuum filtration under Ultrasonic Conditions, and cleaned with distilled water, then dried in vacuum drying chamber, be ground to
200 mesh, obtain final product modified Concave-convex clay rod, wherein, the addition volume of watery hydrochloric acid：Concave convex rod quality is 1mL：5g；
（3）The preparation of polyacrylamide modified graphene：20 parts of graphene oxide is weighed, 20 times of weight of graphene oxide are added
Water, through ultrasonication 30min, adds acrylamide monomer, ammonium persulfate, the stirring reaction 5h under the conditions of 80 DEG C, purification
Obtain the modified graphene oxide of polyacrylamide；
To distilled water is added in modified graphene oxide, adding vitamin C carries out reduction reaction 3h, vacuum filtration, and
Washing, obtains final product polyacrylamide modified graphene；
（4）Modified attapulgite adsorbent：According to proportioning by modified Concave-convex clay rod and polyacrylamide modified graphite
Alkene is added in conical flask, is added water, and is stirred, and is subsequently placed in ultrasound 50min under Ultrasonic Conditions, and then vacuum filtration is put
Dried in vacuum drying chamber, be ground to particle diameter for 200 mesh, obtain final product the modified attapulgite adsorbent.
Step（2）In distillation water cleaning method include：By in the Concave-convex clay rod addition beaker after suction filtration, add and steam
Distilled water, is placed in ultrasound 5min under Ultrasonic Conditions, is repeated 2 times operation.
Step（3）The acrylamide monomer of middle addition is 1 part, and its quality is 20 times of ammonium persulfate quality.
Step（3）Middle washing process is first washed with distillation, and again with methanol is washed, then is washed with distillation, can fully be washed
Adsorb the acrylamide and polyacrylamide and other impurities in graphenic surface.
Modified attapulgite earth adsorbing is applied to the treatment of waste water, and step is as follows：
The modified attapulgite earth adsorbing for preparing is taken respectively to be added in 500mL waste water, wherein, Pb is contained in waste water2+, Cu2 +, Cd2+Ion, wherein the concentration of each ion is 20mg/L, adds modified attapulgite earth adsorbing, in the rotating speed of 250 turns/min
Under the conditions of, the clearance of each metal see the table below with the relational result of the addition of adsorbent after adsorption time 2h：
In sum, the attapulgite clay adsorbent that the present invention is prepared is due to excellent dispersing uniformity so that make
During micro use can heavy metal ion preferable suction-operated, with preferable adsorption and sedimentation efficiency, significantly
Use cost is reduced, for the safety dumping of waste water provides guarantee, it is to avoid because wastewater treatment caused environment not up to standard is dirty
Dye, while the cost of wastewater treatment is reduced, with preferable application value.Additionally, the preparation method is simple, condition temperature
With, it is time-consuming short, be adapted to industrial production.
Specific embodiment of the invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can within the scope of the claims make various deformations or amendments, this not shadow
Sound substance of the invention.
Claims (10)
1. a kind of modified attapulgite earth adsorbing, it is characterised in that：Each component including following parts by weight：Modified attapulgite
20 ~ 40 parts of clay, 10 ~ 20 parts of polyacrylamide modified graphene, also including appropriate solvent.
2. modified attapulgite earth adsorbing according to claim 1, it is characterised in that：The modified attapulgite clay is
The modified Concave-convex clay rod of acid.
3. modified attapulgite earth adsorbing according to claim 1, it is characterised in that：The solvent includes first alcohol and water.
4. the method that one kind prepares the modified attapulgite earth adsorbing as described in any one of claim 1 ~ 3, it is characterised in that：Bag
Include following steps：
（1）The pretreatment of Concave-convex clay rod：Natural attapulgite clay is carried out to be crushed to 100 ~ 200 mesh, is added water, stir shape
Into mud in suspension, then by ultrasound it is fully dispersed after, take upper suspension in the centrifuge of 3000 turns/min centrifugal treating 5 ~
10min, vacuum filtration obtains Concave-convex clay rod one after standing；
Concave-convex clay rod one is placed in beaker, methyl alcohol is added, in 10 ~ 20min of ultrasound, vacuum after standing under Ultrasonic Conditions
Suction filtration, is dried to obtain Concave-convex clay rod two；
（2）The preparation of modified attapulgite clay：Concave-convex clay rod two is placed in flask, the watery hydrochloric acid of 2mol/L is added,
In 10 ~ 20min of ultrasound, vacuum filtration under Ultrasonic Conditions, and cleaned with distilled water, then dried in vacuum drying chamber, ground
100 ~ 200 mesh are milled to, modified Concave-convex clay rod is obtained final product；
（3）The preparation of polyacrylamide modified graphene：10 ~ 20 parts of graphene oxide is weighed, 10 ~ 20 times of graphene oxide is added
The water of weight, through 20 ~ 30min of ultrasonication, adds acrylamide monomer, ammonium persulfate, is stirred under the conditions of 80 DEG C ~ 90 DEG C
3 ~ 5h of reaction is mixed, purification obtains the modified graphene oxide of polyacrylamide；
To distilled water is added in modified graphene oxide, adding vitamin C carries out 2 ~ 3h of reduction reaction, vacuum filtration,
And wash, obtain final product polyacrylamide modified graphene；
（4）Modified attapulgite adsorbent：According to proportioning by modified Concave-convex clay rod and polyacrylamide modified graphite
Alkene is added in conical flask, is added water, and is stirred, and is subsequently placed in 30 ~ 50min of ultrasound under Ultrasonic Conditions, vacuum filtration, then
It is placed in vacuum drying chamber and dries, be ground to particle diameter for 100 ~ 200 mesh, obtains final product the modified attapulgite adsorbent.
5. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（1）
In the weight that adds water be 3 ~ 8 times of Concave-convex clay rod weight.
6. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（1）
The addition volume of middle methyl alcohol is 50mL with Concave-convex clay rod mass ratio：5~10g.
7. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（2）
The addition volume of middle watery hydrochloric acid：Concave convex rod quality is 1mL：2g~5g.
8. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（2）
In distillation water cleaning method include：By in the Concave-convex clay rod addition beaker after suction filtration, distilled water is added, be placed in ultrasonic wave
Under the conditions of ultrasound 5min, be repeated 2 times operation.
9. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（3）
The acrylamide monomer of middle addition is 0.1 ~ 1 part, and its quality is 10 ~ 20 times of ammonium persulfate quality.
10. the preparation method of modified attapulgite earth adsorbing according to claim 4, it is characterised in that：The step（3）
Middle washing process is first washed with distillation, and again with methanol is washed, then is washed with distillation.
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