CN105921108A - Preparation method and application of montmorillonoid and carbon composite material - Google Patents
Preparation method and application of montmorillonoid and carbon composite material Download PDFInfo
- Publication number
- CN105921108A CN105921108A CN201610365980.4A CN201610365980A CN105921108A CN 105921108 A CN105921108 A CN 105921108A CN 201610365980 A CN201610365980 A CN 201610365980A CN 105921108 A CN105921108 A CN 105921108A
- Authority
- CN
- China
- Prior art keywords
- montmorillonite
- carbon composite
- deionized water
- temperature
- serosity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method and application of a montmorillonite and carbon composite material. According to the method, low-cost and highly-available montmorillonite and dextrose monohydrate are taken as raw materials, and the surface of a composite material is modified by the steps of purification and sodium modification of the montmorillonite, hydrothermal treatment of the montmorillonite and the dextrose monohydrate, functionalization of the composite material and the like, so as to prepare carbon modified montmorillonite for water treatment. The montmorillonite and carbon composite material obtained by the method has high stability and adsorption performance, and the maximum adsorption capacity for lead ions in wastewater is 932.49mg/g; according to the method, the adsorption performance of the montmorillonite for heavy metals can be effectively improved, separation effects are improved, and recovery can be realized; a preparation condition is mild and simple, and the montmorillonite and carbon composite material is an efficient and low-cost heavy metal ion adsorbent.
Description
Technical field
Invention belongs to the crossing domain of environment and material, is specifically related to preparation and the application of the composite of a kind of montmorillonite and carbon.
Background technology
During the nearly last ten years, along with the continuous acceleration of Chinese Industrialization, the industry relating to heavy metals emission gets more and more, including ore deposit
Mountain exploitation, metal smelt, chemical industry, printing and dyeing, leather, pesticide, feedstuff etc., add some contaminating enterprises illegal exploitation,
Exceed standard the problems such as blowdown, makes heavy metal pollution event situation occurred frequently occur.The fast development of industry causes substantial amounts of heavy metal to enter
Environment, these heavy metal contaminants cause the most serious harm to environment and human health.Heavy metal wastewater thereby is essentially from ore deposit
Hole, mountain internal drainage, waste-rock yard drench immersion, the dedusting draining of mill tailings draining non-ferrous metals smelting works, Non-ferrous Metals Processing Factory's acid
Wash water, Electroplate Factory's plating piece washings, steel plant's pickling draining, and electrolysis, pesticide, medicine, Nicotiana tabacum L., paint, pigment etc.
Industry.
Owing to heavy metal can not be decomposed for Institute of Micro-biology, and it is prone to by food chain at people's body accumulation, is converted into toxicity bigger
Methyl compound, will cause serious threat to health after exceeding finite concentration.Such as, mantoquita has bigger poison to human body
Property, can cause hepatorenal damage, moreover it is possible to damaged cells red blood and cause intravascular hemolysis.Lead is to act on each system of Whole Body and device
The cumulative toxicant of official, main accumulation, in system and kidneys such as nerve, hemopoietic, digestion, cardiovascular, damages medulla hematopoietic system
With nervous system etc..At the beginning of 2011, " heavy metal pollution integrated control " 12 " planning " obtains State Council's reply, this
It is in the planning that China includes the preventing and treating of heavy metal pollution in country in history for the first time.According to planning requirement, by 2015,
The discharge of the heavy metal contaminants such as key area lead, hydrargyrum, chromium and arsenic, cut down 15% than 2007.By 2015, emphasis
Region, emphasis heavy metal pollution discharge capacity reduced 15% than 2007, and the emphasis heavy metal pollution discharge capacity of non-key area is not
Level more than 2007.Therefore, heavy metal pollution of water body arouses great concern.
By front described, lead waste water pollutes environment, is detrimental to health, develop cheap, choose, regenerating easily be
Row water treatment and purification new material becomes the focus of research and development at present.Absorption method remain process heavy metal wastewater thereby main method it
One.But adsorbent somewhat expensive is the main cause of its application of restriction.In recent years, montmorillonite as a kind of new adsorbent at water
Process aspect is applied, but its difficult separation characteristic in water body constrains its utilization.China's montmorillonite aboundresources, comes
Source is wide, low cost, and montmorillonite/carbon composite has specific surface area greatly, and the feature that absorption property is good, as suction
Remove heavy metal ions in wastewater for attached dose and there is great social benefit and environmental benefit.
Summary of the invention
Present invention aim at, it is provided that a kind of montmorillonite and the preparation method and application of carbon composite, the method utilizes cheap easy
Montmorillonite and Dextrose Monohydrate be raw material, by purification and the sodium of montmorillonite, montmorillonite and the hydrothermal treatment consists of glucose and
The step modifying surfaces to composite such as composite official energy dough, thus complete the system of water process carbon modified montmorillonoid
Standby.The montmorillonite obtained by the method for the invention and carbon composite good stability, absorption property are good, to lead in sewage from
Sub-maximal absorptive capacity is 932.49mg/g, and the method can be effectively improved the absorption property of montmorillonite heavy metal, and separate effect
Fruit is improved, recyclable, preparation condition is gentle, simple, is a kind of efficient, inexpensive adsorbent for heavy metal.
A kind of montmorillonite of the present invention and the preparation method of carbon composite, carried out montmorillonite and glucose at physical chemistry
Reason, synthesizes montmorillonite/carbon composite, then it is modified that its composite material surface carries out sense dough, and following step is pressed in concrete operations
Suddenly carry out:
A kind of montmorillonite and the preparation method of carbon composite, it is characterised in that montmorillonite and glucose are carried out at physical chemistry
Reason, synthesis montmorillonite and carbon composite, then it is modified that its composite material surface carries out sense dough, following step is pressed in concrete operations
Suddenly carry out:
A, the purification of montmorillonite and sodium: take in montmorillonite addition deionized water and stir, then stand, after being layered,
Bottom residues being poured out, stay the supernatant stand-by, so circulation 4 times, prepares and purifies montmorillonite, and the montmorillonite after purifying adds
Enter deionized water and be slowly stirred the uniform mixed liquor of formation, be subsequently adding solid sodium chloride, the continuously stirred serosity being uniformly mixed,
Again by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion, be finally dried to obtain sodio and cover de-
Soil；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite in step a and add deionized water, supersound process half
Hour, form uniform mixed liquor, in mixed liquor, add Dextrose Monohydrate, vigorous magnetic stirring 50min, be uniformly mixed
Serosity, the serosity obtained is poured in water heating kettle, close good after, water heating kettle is put into temperature 160-200 DEG C reaction in baking oven
24 hours, then mixture is filtered, deionized water rinsing 4 times, remove the impurity such as glucose, temperature 80 DEG C is dried, and mills
Rear mistake 200 mesh sieve, obtains montmorillonite and carbon composite, and wherein montmorillonite and Dextrose Monohydrate mass ratio are 1:0.5-1:4；
Prepared by c, the montmorillonite of sense dough and carbon composite: weigh montmorillonite and carbon composite in step b, adds matter
Amount mark is in the hydrogen peroxide 50mL of 10%-30%, after being stirred vigorously 4.0 hours, and centrifugation, it is washed with deionized water 3 times,
Temperature 60 C is dried and is obtained carboxylated montmorillonite and carbon composite；
Or montmorillonite and carbon composite are mixed with the NaOH solution that concentration is 0.1-1.0mol/L, it is then transferred into reaction
In still, hot water reaction 5h at temperature 150 DEG C, repeatedly cleans with deionized water, is dried, obtain hydroxylated montmorillonite and carbon is multiple
Condensation material；
Or in 50mL ethylenediamine solution, add montmorillonite and carbon composite and sodium nitrite, by mixed liquor at temperature 50 C water
Ultrasonic half an hour under bath temperature, then microwave treatment 40min at temperature is 80-100 DEG C, eventually passes and repeatedly rinses product,
It is dried, obtains amidized montmorillonite and carbon composite.
Montmorillonite and carbon composite that described method obtains are removing the purposes contained in heavy metal lead ion sewage.
A kind of montmorillonite of the present invention and the preparation method and application of carbon composite, to the montmorillonite before and after sense dough and
The carbon composite performance evaluation to lead containing wastewater treatment: montmorillonite and carbon composite, carboxylated montmorillonite and carbon will be obtained
Composite, hydroxylated montmorillonite and carbon composite and amidized montmorillonite/carbon composite 0.4g/L are added to leaded
In waste water 10-300mg/L, being then adjusted to pH is 6 and temperature 303K, carries out waste water vibrating 27 hours under 150rpm,
After separation, the performance evaluation of Adsorption heavy metal lead ion can be carried out.
A kind of montmorillonite of the present invention and the preparation method of carbon composite, the method introducing by carbon, improves further
The functional group densities on its surface, thus substantially increase the absorbability of heavy metal ion.To obtain montmorillonite and carbon composite wood
Material, carboxylated montmorillonite and carbon composite, hydroxylated montmorillonite and carbon composite and amidized montmorillonite and carbon are again
Condensation material is adsorbent, and the lead to variable concentrations carries out adsorption test respectively, and adsorbent dosage is 0.4g/L, and lead ion is dense
Degree is 2-7 for 10-300mg/L, pH, and temperature is 15-30 DEG C, and adsorption time is 27 hours.Its result shows: montmorillonite
With carbon and carboxylated montmorillonite and carbon, the adsorbance maximum of lead ion be can reach 702.82 and 932.49mg/g, be much higher than illiteracy
De-soil and the activated carbon absorbability to lead ion.Meanwhile, preparation montmorillonite and carbon composite, montmorillonite and a carbon source (water
Glucose) mass ratio can reach optimal implementation result in the range of 1:0.5-4, and increase carbon source amount and can improve absorption effect
Really, but too much carbon source can reduce absorbability.
In sum, adsorbent for heavy metal of the present invention not only raw material is cheap, be easy to get, and preparation is simple, and counterweight
Metallic lead ion has good removal effect.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph preparing montmorillonite/carbon composite in the embodiment of the present invention 5；
Fig. 2 is change to lead ion adsorbance under different montmorillonites and carbon source mass ratio in the present invention, and wherein lead ion is initial
Concentration is 200mg/L；
Fig. 3 is change to the adsorbance of lead ion under different hydrothermal temperatures, wherein montmorillonite and carbon source quality in the present invention
Ratio be 1:3.7.
Fig. 4 is the change to lead ion adsorbance of the adsorbent of different functional groups of the present invention, and wherein lead ion initial concentration is
300mg/L；
Fig. 5 is the change to lead ion clearance of the adsorbent of different functional groups of the present invention, and wherein lead ion initial concentration is
300mg/L。
Detailed description of the invention:
Embodiment 1 (montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in 20g montmorillonite addition 400mL deionization and stir, then stand, treat
After layering, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will cover
De-soil adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1g, continuously stirred
To the serosity of mix homogeneously, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
After be dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite in step a and add deionized water, supersound process half
Hour, forming uniform mixed liquor, be that 1:0.5-1:4 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking oven
Middle temperature 160-200 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
The montmorillonite obtained and carbon composite 0.4g/L are added in leaded 200mg/L sewage, are then adjusted to pH=6
With temperature 288K, carry out sewage vibrating 27 hours under 150rpm, after separation, water sample after processing is measured, with table
Mode enumerate:
Table 1
| Sequence number | Montmorillonite | Dextrose Monohydrate | Temperature DEG C | Lead ion surplus (mg/L) | Adsorbance (mg/g) |
| 1 | 1 | 0.5 | 200 | 49.62 | 375.96 |
| 2 | 1 | 1 | 200 | 47.75 | 380.62 |
| 3 | 1 | 2 | 200 | 16.02 | 459.95 |
| 4 | 1 | 3 | 200 | 7.28 | 481.80 |
| 5 | 1 | 3.7 | 200 | 7.02 | 482.45 |
| 6 | 1 | 4 | 200 | 17.96 | 455.11 |
| 7 | 1 | 3.7 | 160 | 141.4 | 146.50 |
| 8 | 1 | 3.7 | 180 | 47.02 | 382.45 |
| 9 | 1 | 3.7 | 200 | 38.83 | 407.93 |
Embodiment 10
Montmorillonite and the carbon composite adsorbent 0.4g/L of preparation in embodiment 5 are added in leaded 300mg/L sewage,
It is then adjusted to pH=6 and temperature 303K, carries out sewage vibrating 27 hours under 150rpm, after separation, i.e. can reach absorption
Remove the purpose of heavy metal lead ion.Being measured water sample after processing, the adsorbance of this adsorbent is 550.00mg/g, lead
Ion remaval rate is 73.30%.
Embodiment 11 (carboxylated montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, form uniform mixed liquor, be that 1:3.7 adds Dextrose Monohydrate, vigorous magnetic in mixed liquor in mass ratio
Stirring 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into
In baking oven, temperature 200 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: weigh montmorillonite and carbon composite in step b, join
Mass fraction is in the hydrogen peroxide 50mL of 30%, after being stirred vigorously 4.0 hours, and centrifugation, it is washed with deionized water 3 times,
Temperature 60 C is dried and is obtained carboxylated montmorillonite and carbon composite；
Carboxylated montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, so
After be adjusted to pH=6 and temperature 303K, sewage is carried out under 150rpm vibrate 27 hours, after separation, i.e. can reach absorption and go
The purpose of removing heavy metals lead ion.Being measured water sample after processing, the adsorbance calculating this adsorbent is 696.00mg/g,
Lead ion clearance is 92.80%.
Embodiment 12 (carboxylated montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:3 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 180 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: weigh montmorillonite and carbon composite in step b, join
Mass fraction is in the hydrogen peroxide 50mL of 10%, after being stirred vigorously 4.0 hours, and centrifugation, it is washed with deionized water 3 times,
Temperature 60 C is dried and is obtained carboxylated montmorillonite and carbon composite；
Carboxylated montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, so
After be adjusted to pH=6 and temperature 303K, sewage is carried out under 150rpm vibrate 27 hours, after separation, i.e. can reach absorption and go
The purpose of removing heavy metals lead ion.Being measured water sample after processing, the adsorbance calculating this adsorbent is 696.00mg/g,
Lead ion clearance is 92.80%.
Embodiment 13 (carboxylated montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:4 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 200 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: weigh montmorillonite/carbon composite in step b, join matter
Amount mark is in the hydrogen peroxide 50mL of 20%, after being stirred vigorously 4.0 hours, and centrifugation, it is washed with deionized water 3 times, temperature
Spend 60 DEG C of drying and obtain carboxylated montmorillonite and carbon composite；
Carboxylated montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, so
After be adjusted to pH=6 and temperature 303K, sewage is carried out under 150rpm vibrate 27 hours, after separation, i.e. can reach absorption and go
The purpose of removing heavy metals lead ion.Being measured water sample after processing, the adsorbance calculating this adsorbent is 696.00mg/g,
Lead ion clearance is 92.80%.
Embodiment 15 (hydroxylating montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:1 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 160 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: by 3.0g montmorillonite/carbon composite with 50mL concentration be
The NaOH solution mixing of 0.1mol/L, is then transferred in reactor, hot water reaction 5h at temperature 150 DEG C, uses deionized water
Repeatedly clean, be dried, obtain hydroxylated montmorillonite and carbon composite；
Hydroxylated montmorillonite and the carbon composite 0.4g/L of preparation are added in leaded 300mg/L sewage, then regulate
To pH=6 and temperature 303K, carry out sewage vibrating 27 hours under 150rpm, after separation, water sample after processing be measured,
The adsorbance calculating this adsorbent is 661.70mg/g, and lead ion clearance is 88.20%.Reach Adsorption heavy metal lead
The purpose of ion.
Embodiment 16 (hydroxylating montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
B, the preparation of montmorillonite/carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, ultrasonic
Processing half an hour, form uniform mixed liquor, be that 1:2 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking oven
Middle temperature 180 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose, temperature
Spend 80 DEG C to be dried, cross 200 mesh sieves after milling, obtain montmorillonite and carbon composite；
Prepared by c, the montmorillonite of sense dough and carbon composite: by 3.0g montmorillonite and carbon composite with concentration be
The NaOH solution mixing of 0.5mol/L, is then transferred in reactor, hot water reaction 5h at temperature 150 DEG C, uses deionized water
Repeatedly clean, be dried, obtain hydroxylated montmorillonite and carbon composite；
Hydroxylated montmorillonite and the carbon composite 0.4g/L of preparation are added in leaded 300mg/L sewage, then regulate
To pH=6 and temperature 303K, carry out sewage vibrating 27 hours under 150rpm, after separation, water sample after processing be measured,
The adsorbance calculating this adsorbent is 661.70mg/g, and lead ion clearance is 88.20%.
Embodiment 17 (hydroxylating montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:4 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 200 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: by 3.0g montmorillonite and carbon composite with concentration be
The NaOH solution mixing of 1.0mol/L, is then transferred in reactor, hot water reaction 5h at temperature 150 DEG C, uses deionized water
Repeatedly clean, be dried, obtain hydroxylated montmorillonite and carbon composite；
Hydroxylated montmorillonite and the carbon composite 0.4g/L of preparation are added in leaded 300mg/L sewage, then regulate
To pH=6 and temperature 303K, carry out sewage vibrating 27 hours under 150rpm, after separation, water sample after processing be measured,
The adsorbance calculating this adsorbent is 661.70mg/g, and lead ion clearance is 88.20%.
Embodiment 18 (amidized montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, form uniform mixed liquor, be that 1:0.5 adds Dextrose Monohydrate, vigorous magnetic in mixed liquor in mass ratio
Stirring 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into
In baking oven, temperature 180 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: add 3.0g montmorillonite/carbon in 50mL ethylenediamine solution multiple
Condensation material and sodium nitrite 2.0g, by mixed liquor ultrasonic half an hour under temperature 50 C bath temperature, be then 80 DEG C in temperature
Lower microwave treatment 40min, eventually passes and repeatedly rinses product, is dried, obtains amidized montmorillonite/carbon composite；
Amidized montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, adjust
Sewage, to pH=6 and temperature 303K, is carried out vibrating 27 hours under 150rpm by joint, after separation, surveys water sample after processing
Fixed, the adsorbance calculating this adsorbent is 602.40mg/g, and lead ion clearance is 80.30% (such as Fig. 4), i.e. can reach
The purpose of Adsorption heavy metal lead ion.
Embodiment 19 (amidized montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:3 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 170 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: add 3.0g montmorillonite/carbon in 50mL ethylenediamine solution multiple
Condensation material and NaNO22.0g, by mixed liquor ultrasonic half an hour under temperature 50 C bath temperature, then at temperature is 100 DEG C
Microwave treatment 40min, eventually passes and repeatedly rinses product, is dried, obtains amidized montmorillonite/carbon composite；
Amidized montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, adjust
Sewage, to pH=6 and temperature 303K, is carried out vibrating 27 hours under 150rpm by joint, after separation, surveys water sample after processing
Fixed, the adsorbance calculating this adsorbent is 602.40mg/g, and lead ion clearance is 80.30% (such as Fig. 4), i.e. can reach
The purpose of Adsorption heavy metal lead ion.
Embodiment 20 (amidized montmorillonite and carbon composite)
A, the purification of montmorillonite and sodium: take in the montmorillonite addition 200mL deionized water of 10g and stir, then stand,
After being layered, bottom residues being poured out, the supernatant is continuing with, and so circulation 4 times, prepares the montmorillonite of higher degree, will
Montmorillonite adds 100mL deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride 1.0g, persistently stirs
Mix the serosity being uniformly mixed, then by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion,
Finally it is dried to obtain sodium-based montmorillonite；
The preparation of b, montmorillonite and carbon composite: weigh sodium-based montmorillonite 2g in step a and add 20mL deionized water, super
Sonication half an hour, forming uniform mixed liquor, be that 1:4 adds Dextrose Monohydrate in mixed liquor in mass ratio, vigorous magnetic stirs
Mix 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into baking
In case, temperature 190 DEG C is reacted 24 hours, then is filtered by mixture, deionized water rinsing 4 times, removes the impurity such as glucose,
Temperature 80 DEG C is dried, and crosses 200 mesh sieves, obtain montmorillonite and carbon composite after milling；
Prepared by c, the montmorillonite of sense dough and carbon composite: add 3.0g montmorillonite/carbon in 50mL ethylenediamine solution multiple
Condensation material and NaNO22.0g, by mixed liquor ultrasonic half an hour under temperature 50 C bath temperature, then at temperature is 90 DEG C
Microwave treatment 40min, eventually passes and repeatedly rinses product, is dried, obtains amidized montmorillonite and carbon composite；
Amidized montmorillonite and the carbon composite adsorbent 0.4g/L of preparation are added in leaded 300mg/L sewage, adjust
Sewage, to pH=6 and temperature 303K, is carried out vibrating 27 hours under 150rpm by joint, after separation, surveys water sample after processing
Fixed, the adsorbance calculating this adsorbent is 602.40mg/g, and lead ion clearance is 80.30% (such as Fig. 4), i.e. can reach
The purpose of Adsorption heavy metal lead ion.
Embodiment 21
Montmorillonite and the carbon composite 0.4g/L of preparation in embodiment 5 are added in leaded 10-200mg/L sewage, then
It is adjusted to pH=6 and temperature 303K, carries out waste water vibrating 27 hours under 150rpm, after separation, water sample after processing is carried out
Measure, last result is simulated Langmuir adsorption isotherm, Langmuir model obtains its maximum to lead ion
Adsorbance is 702.82mg/g (table 2).
Embodiment 22
It is dirty that carboxylated montmorillonite embodiment 11-13 prepared and carbon composite 0.4g/L are added to leaded 10-200mg/L
In water, it is then adjusted to pH=6 and temperature 303K, carries out sewage vibrating 27 hours, after separation, to process under 150rpm
Rear water sample is measured, and last result is simulated Langmuir adsorption isotherm, Langmuir model obtain it to lead
The maximal absorptive capacity of ion is 932.49mg/g (table 2):
The Langmuir Adsorption Model parameter that lead ion is adsorbed by table 2 montmorillonites/carbon and carboxylated montmorillonite/carbon
As can be seen from the table: montmorillonite/carbon and carboxylated montmorillonite/carbon are respectively 702.82 Hes to the maximal absorptive capacity of lead ion
932.49mg/g, has good removal effect to leaded sewage.
Claims (2)
1. a montmorillonite and the preparation method of carbon composite, it is characterized in that montmorillonite and glucose are carried out physical chemistry process, synthesis montmorillonite and carbon composite, then it is modified that its composite material surface carries out sense dough, concrete operations follow these steps to carry out:
A, the purification of montmorillonite and sodium: take in montmorillonite addition deionized water and stir, then stand, after being layered, bottom residues is poured out, stay the supernatant stand-by, so circulation 4 times, prepare and purify montmorillonite, montmorillonite after purifying adds deionized water and is slowly stirred the uniform mixed liquor of formation, is subsequently adding solid sodium chloride, the continuously stirred serosity being uniformly mixed, again by serosity centrifugal treating, add deionized water, be cleaned multiple times till cleaning chloride ion, be finally dried to obtain sodium-based montmorillonite；
B, montmorillonite and the preparation of carbon composite: weigh sodium-based montmorillonite in step a and add deionized water, supersound process half an hour, form uniform mixed liquor, Dextrose Monohydrate is added in mixed liquor, vigorous magnetic stirring 50min, the serosity being uniformly mixed, the serosity obtained is poured in water heating kettle, after closing well, water heating kettle is put into temperature 160-200 DEG C in baking oven react 24 hours, again mixture is filtered, deionized water rinsing 4 times, remove the impurity such as glucose, temperature 80 DEG C is dried, 200 mesh sieves are crossed after milling, obtain montmorillonite and carbon composite, wherein montmorillonite and Dextrose Monohydrate mass ratio are 1:0.5-1:4；
Prepared by c, the montmorillonite of sense dough and carbon composite: weigh montmorillonite and carbon composite in step b, add in the hydrogen peroxide 50mL that mass fraction is 10%-30%, after being stirred vigorously 4.0 hours, centrifugation, being washed with deionized water 3 times, temperature 60 C is dried and is obtained carboxylated montmorillonite and carbon composite；
Or montmorillonite and carbon composite are mixed with the NaOH solution that concentration is 0.1-1.0mol/L, it is then transferred in reactor, hot water reaction 5h at temperature 150 DEG C, repeatedly cleans with deionized water, be dried, obtain hydroxylated montmorillonite and carbon composite；
Or in 50mL ethylenediamine solution, add montmorillonite and carbon composite and sodium nitrite, by mixed liquor ultrasonic half an hour under temperature 50 C bath temperature, then microwave treatment 40min at temperature is 80-100 DEG C, eventually pass and repeatedly rinse product, it is dried, obtains amidized montmorillonite and carbon composite.
Montmorillonite and carbon composite that the most according to claim 1, method obtains are removing the purposes contained in heavy metal lead ion sewage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610365980.4A CN105921108A (en) | 2016-05-28 | 2016-05-28 | Preparation method and application of montmorillonoid and carbon composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610365980.4A CN105921108A (en) | 2016-05-28 | 2016-05-28 | Preparation method and application of montmorillonoid and carbon composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105921108A true CN105921108A (en) | 2016-09-07 |
Family
ID=56841416
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610365980.4A Pending CN105921108A (en) | 2016-05-28 | 2016-05-28 | Preparation method and application of montmorillonoid and carbon composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105921108A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311147A (en) * | 2016-10-17 | 2017-01-11 | 中国矿业大学(北京) | Illite loaded nanocarbon compound adsorbing material and preparation method thereof |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN108212088A (en) * | 2018-01-26 | 2018-06-29 | 中国科学院烟台海岸带研究所 | Nano-sized carbon-montmorillonite composite material and the permeable reactive barrier structure filled with the material |
| CN108236925A (en) * | 2016-12-27 | 2018-07-03 | 海门市源美美术图案设计有限公司 | A kind of bentonite nano carbon composite and its application |
| CN109420481A (en) * | 2017-08-29 | 2019-03-05 | 钱诗旋 | A kind of modified MMT/C nano-complex and preparation method thereof |
| CN109517354A (en) * | 2018-11-22 | 2019-03-26 | 安徽汇创新材料有限公司 | A kind of fire-retardant resistance to compression composite material and preparation method for glass toughening manure pit |
| CN110496593A (en) * | 2018-05-18 | 2019-11-26 | 南京理工大学 | Lamellar graphite phase carbon nitride/montmorillonite composite material and its preparation method and application |
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | Compound adsorbent and the preparation method and application thereof |
| CN117384474A (en) * | 2023-10-27 | 2024-01-12 | 佛山安亿纳米材料有限公司 | High-strength composite film and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752269A (en) * | 2014-01-23 | 2014-04-30 | 河海大学 | Modified active carbon and preparation method thereof |
-
2016
- 2016-05-28 CN CN201610365980.4A patent/CN105921108A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103752269A (en) * | 2014-01-23 | 2014-04-30 | 河海大学 | Modified active carbon and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| A. AMIRI等: "One-pot, efficient functionalization of multi-walled carbon nanotubes with diamines by microwave method", 《APPLIED SURFACE SCIENCE》 * |
| 刘宏燕: "椰壳基活性炭改性及其对Pb2+的吸附性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 张佳: "中孔活性炭的化学改性及其对Pb2+的吸附性能的研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 李铁: "新型碳基功能材料的制备、表征及其应用研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106311147A (en) * | 2016-10-17 | 2017-01-11 | 中国矿业大学(北京) | Illite loaded nanocarbon compound adsorbing material and preparation method thereof |
| CN108236925A (en) * | 2016-12-27 | 2018-07-03 | 海门市源美美术图案设计有限公司 | A kind of bentonite nano carbon composite and its application |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN109420481A (en) * | 2017-08-29 | 2019-03-05 | 钱诗旋 | A kind of modified MMT/C nano-complex and preparation method thereof |
| CN108212088A (en) * | 2018-01-26 | 2018-06-29 | 中国科学院烟台海岸带研究所 | Nano-sized carbon-montmorillonite composite material and the permeable reactive barrier structure filled with the material |
| CN110496593A (en) * | 2018-05-18 | 2019-11-26 | 南京理工大学 | Lamellar graphite phase carbon nitride/montmorillonite composite material and its preparation method and application |
| CN109517354A (en) * | 2018-11-22 | 2019-03-26 | 安徽汇创新材料有限公司 | A kind of fire-retardant resistance to compression composite material and preparation method for glass toughening manure pit |
| CN110496599A (en) * | 2019-07-25 | 2019-11-26 | 南方科技大学 | Compound adsorbent and the preparation method and application thereof |
| CN110496599B (en) * | 2019-07-25 | 2022-08-23 | 南方科技大学 | Composite adsorbent and preparation method and application thereof |
| CN117384474A (en) * | 2023-10-27 | 2024-01-12 | 佛山安亿纳米材料有限公司 | High-strength composite film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105921108A (en) | Preparation method and application of montmorillonoid and carbon composite material | |
| CN106179202A (en) | A kind of composite modified biological carbon materials of iron-based amino and preparation and application | |
| CN105558763A (en) | Method for reducing content of heavy metals in grains | |
| CN106179247A (en) | A kind of Cr VI adsorbent and its preparation method and application | |
| CN103623782A (en) | Preparation method for composite magnetic adsorption material and method for removing heavy metal ions in waste water | |
| CN103071463A (en) | Modified peanut shell Pb(II) adsorbent, and preparation method and application thereof | |
| CN108793305A (en) | A kind of ammonia nitrogen removal agent | |
| CN105148835B (en) | Granular pattern 13X molecular sieves/attapulgite loaded Nanoscale Iron nickel material and preparation method thereof | |
| CN105771918A (en) | Preparation method and application of magnetic anaerobic granular sludge-chitosan adsorbent | |
| CN106167304A (en) | A kind of heavy metal-polluted water treatment agent and processing method | |
| CN105642368B (en) | A kind of modified TiO2/ CNTs composite catalysts and preparation method thereof | |
| CN102965312A (en) | Modification method for improving bacteria heavy metal adsorption capacity, adsorbent and application thereof | |
| CN107812510A (en) | A kind of composite type water treating agent and preparation method thereof | |
| Ogbozige et al. | Adsorption isotherms and kinetics of lead and cadmium ions: Comparative studies using modified melon (Citrullus colocynthis) husk | |
| CN107694532A (en) | A kind of soil heavy mental adsorbent and preparation method thereof | |
| CN107552015A (en) | A kind of modified mangosteen shell and the method using vanadium in its reduction water body | |
| CN109603768B (en) | Preparation method of economic and reproducible biogas residue-based heavy metal adsorbent | |
| CN207109133U (en) | The quick clean online plating solution negative pressure evaporation equipment for reclaiming of electronickelling production line | |
| CN107149927A (en) | A kind of modified silk fiber prepares the method and its application of heavy-metal adsorption material | |
| CN107119311A (en) | The quick clean online plating solution negative pressure evaporation reuse method of electronickelling production line and equipment | |
| CN108126667A (en) | A kind of flocculant and preparation method thereof | |
| CN108500030A (en) | A kind of Na2The method that EDTA couples heavy metal in Zero-valent Iron removal medical refuse burning flyash | |
| CN105879840A (en) | Organic-inorganic compound and application thereof in water treatment | |
| CN105905952A (en) | Water treatment agent and application thereof | |
| CN105776407A (en) | Environment-friendly sewage treating agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160907 |