CN108786729A - The preparation method of mask graphene/active carbon in-situ plural gel adsorbent - Google Patents
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent Download PDFInfo
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- CN108786729A CN108786729A CN201810573529.0A CN201810573529A CN108786729A CN 108786729 A CN108786729 A CN 108786729A CN 201810573529 A CN201810573529 A CN 201810573529A CN 108786729 A CN108786729 A CN 108786729A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28047—Gels
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Abstract
The invention belongs to functional material preparation field, specially a kind of mask graphene/active carbon in-situ plural gel adsorbent.Activated carbon is ground into 10 μm of powders below first, is then dipped into alkaline reduction pore-creating liquid fully absorbing, filters out material.The activated carbon filtered out is scattered in the graphene oxide solution of high-purity high concentration, it is then placed into the water heating kettle that can be rotated up and down, high temperature hydro-thermal postcooling, discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, and final products are obtained after being then cleaned and dried with pure water.Present invention process is simple and environmentally-friendly, and product adsorption capacity is superior.
Description
Technical field
The invention belongs to functional material preparation fields, compound with graphene/active carbon in-situ more particularly, to a kind of mask
The preparation method of gel adsorber.
Background technology
The mechanism that haze weather generates is very complicated, and chemical composition is also very complicated, may cause a variety of diseases.Meanwhile disease
Poison, germ etc. may be attached on the particulate matter of air, spread the disease.PM2.5 is that harm to the human body is most in atmosphere pollution
Big particulate matter, this particulate matter PM2.5 grain sizes are small, rich in a large amount of poisonous and harmful substances and residence time in an atmosphere it is long,
Fed distance is remote, thus the influence to health and atmosphere quality is big.It is exactly to wear to resist PM2.5 most effective way
It wears masks, and the main function components of mask are filter discs.Filter disc filter effect that be irregular, and being filtered on the market
Grain and bacterium are liable to stick on mask (filter disc) close to the position of mouth and nose, cause the growth of bacterium, form secondary pollution.Cause
This is provided simultaneously with certain antibacterial functions it is necessory to provide a kind of excellent intensive filtration sorbing material.
Graphene can reach 2000m as a kind of emerging material, theoretical specific surface area2/ g or more is a kind of excellent
Different sorbing material.But since graphene sheet layer structure is easy to reunite, form the very low three-dimensional agglomerated materials of porosity.And mesh
Preceding many patents and method all effectively cannot keep or control the size in its aperture of graphene, be only used for dyestuff, organic
The pollutions such as solvent are adsorbed, it is difficult to effectively as air filtration sorbing material.
Invention content
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of mask with graphene/
The preparation method of active carbon in-situ plural gel adsorbent is combined into gel state using graphene oxide and active carbon in-situ,
It is assembled into the sorbing material of three-dimensional porous shape, and is drying and remained in three-dimensional porous state.Meanwhile three-dimensional stone
Black alkene gel also has certain antibacterial action because of graphene-structured feature.
The technical scheme is that：
A kind of preparation method of mask graphene/active carbon in-situ plural gel adsorbent, specific preparation process are：
A. activated carbon is ground into 10 μm of powders below, is then dipped into alkaline reduction pore-creating liquid fully inhaling
It receives, then filters out material；
B. the activated carbon filtered out is scattered in graphene oxide solution, is then placed into the water heating kettle that can be turned upside down
In, it is rotated up and down in water-heat process, cools down after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water,
Finally it is dried to obtain final products.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (a), dipping
Alkaline reduction pore-creating liquid is one or both of the saturated aqueous solution of the ammonium hydroxide of 15~20mol/L, sodium carbonate, potassium carbonate
More than, 10~60min of room temperature immersion time.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (b), oxidation
A concentration of 0.5~2g/L of graphene, conductivity are less than 400 μ s/cm, and graphene oxide is 1 with activated carbon dry ratio:5~
100。
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (b), hydro-thermal
Kettle be rotated up and down it is reverse, rotary speed be 10~60 minutes/circle.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (b), hydro-thermal
160 DEG C~250 DEG C of temperature, hydro-thermal time 240min~600min.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (c), hydro-thermal
The material for finishing releasing is cleaned with pure water, and ejected wash water to conductance is less than 200 μ s/cm and stops cleaning.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in step (c), cleaning
After sample using vacuum drying or vacuum freezedrying.
The preparation method of mask graphene/active carbon in-situ plural gel adsorbent, in gel adsorber
Graphene accounts for 1~5wt%, 900~1200m of specific surface area2/ g, mesoporous accounting 10~30%, micropore accounting 65~85%, remaining
Hole is macropore；Wherein, 0.35~2nm of radius is micropore, and it is mesoporous that radius, which is more than 2nm~50nm, and radius is big more than 50nm
Hole.
Compared with prior art, advantages of the present invention and advantageous effect are：
1, the present invention does holder using activated carbon porous structure, prevents sheet graphene oxide from restoring and reunites, restores simultaneously
Graphene oxide hydro-thermal optimizes the pore structure of sorbing material at porous gel, strengthens adsorption effect.
2, the present invention is reduced to pure aquatic system, environmentally protective without using the hypertoxic substances such as hydrazine hydrate or hydrogen iodide.
3, graphene compound in the present invention also has certain antibacterial action.
Specific implementation mode
In specific implementation process, the present invention is combined into gel using graphene oxide and active carbon in-situ, using including
It is prepared by following steps and technique：
A. activated carbon is ground into 10 μm of powders below, then it is impregnated into alkaline reduction pore-creating liquid at room temperature is
One or more, 10~60min of dip time in the ammonium hydroxide or carbonic acid sodium of 18mol/L, the saturated aqueous solution of potassium carbonate, then
Filter out material；
B. the activated carbon filtered out is scattered in a concentration of 0.5~2g/L, conductivity is less than high-purity high concentration of 400 μ s/cm
Graphene oxide solution in, graphene and activated carbon dry ratio are 1:5~100.It is then placed into the water that can be turned upside down
In hot kettle, water heating kettle rotary speed is to enclose for 10~60 minutes one.160 DEG C~250 DEG C of hydrothermal temperature, hydro-thermal time 240min~
600min is cooled to room temperature after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water
Being less than 200 μ s/cm to conductance can stop cleaning, and finally vacuum drying or vacuum freezedrying can be used to obtain final products.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
In the present embodiment, mask is as follows with the preparation method of graphene/active carbon in-situ plural gel adsorbent：
A., activated carbon is ground into 10 μm of 100 grams of powder, then it is impregnated into alkaline reduction pore-creating liquid at room temperature is
In the aqueous solution of the ammonium hydroxide of 18mol/L, then dip time 20min filters out material；
B., the activated carbon filtered out is scattered in the oxidation stone of the high-purity high concentrations of 1L of a concentration of 1g/L, 300 μ s/cm of conductivity
In black alkene solution, graphene oxide is 1 with activated carbon dry ratio:100.It is then placed into the water heating kettle that can be turned upside down,
Water heating kettle rotary speed is to enclose for 50 minutes one.180 DEG C of hydrothermal temperature, hydro-thermal time 300min, is cooled to room temperature after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water
Stop cleaning to 100 μ s/cm of conductance, finally vacuum drying or vacuum freezedrying can be used to obtain final products.
It is characterized by testing, graphene accounts for about 1wt%, product specific surface area 1200m in product2/ g, mesoporous accounting
10.5%, micropore accounting 82.4%, remaining hole is that (0.35~2nm of radius is micropore to macropore, during radius 2nm~50nm is
Hole, it is macropore that radius, which is more than 50nm).
Embodiment 2
In the present embodiment, mask is as follows with the preparation method of graphene/active carbon in-situ plural gel adsorbent：
A., activated carbon is ground into 10 μm of 100 grams of powder, then it is impregnated into alkaline reduction pore-creating liquid at room temperature is
In the aqueous solution of the sodium carbonate of 18mol/L, then dip time 10min filters out material；
B., the activated carbon filtered out is scattered in the oxidation stone of the high-purity high concentrations of 2L of a concentration of 2g/L, 300 μ s/cm of conductivity
In black alkene solution, graphene oxide is 1 with activated carbon dry ratio:60.It is then placed into the water heating kettle that can be turned upside down, water
Hot kettle rotary speed is to enclose for 30 minutes one.200 DEG C of hydrothermal temperature, hydro-thermal time 360min, is cooled to room temperature after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water
Stop cleaning to 150 μ s/cm of conductance, finally vacuum drying or vacuum freezedrying can be used to obtain final products.
It is characterized by testing, graphene accounts for about 4wt%, product specific surface area 900m in product2/ g, mesoporous accounting
25.5%, micropore accounting 67.1%, remaining hole is macropore.
Embodiment 3
In the present embodiment, mask is as follows with the preparation method of graphene/active carbon in-situ plural gel adsorbent：
A., activated carbon is ground into 10 μm of 100 grams of powder, then it is impregnated into alkaline reduction pore-creating liquid at room temperature is
In the aqueous solution of the potassium carbonate of 18mol/L, then dip time 25min filters out material；
B., the activated carbon filtered out is scattered in the oxidation of the high-purity high concentrations of 2L of a concentration of 1.5g/L, 300 μ s/cm of conductivity
In graphene solution, graphene oxide is 1 with activated carbon dry ratio:30.It is then placed into the water heating kettle that can be turned upside down,
Water heating kettle rotary speed is to enclose for 20 minutes one.210 DEG C of hydrothermal temperature, hydro-thermal time 240min, is cooled to room temperature after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water
Stop cleaning to 100 μ s/cm of conductance, finally vacuum drying or vacuum freezedrying can be used to obtain final products.
It is characterized by testing, graphene accounts for about 3wt%, product specific surface area 1021m in product2/ g, mesoporous accounting
12.5%, micropore accounting 77.6%, remaining hole is macropore.
Embodiment the result shows that, the activated carbon filtered out is scattered in the graphene oxide solution of high-purity high concentration by the present invention
In, it is then placed into the water heating kettle that can be rotated up and down, high temperature hydro-thermal postcooling, the graphene oxide that is heat-treated of discharging water/
Active carbon in-situ plural gel adsorbent, final products are obtained after being then cleaned and dried with pure water.This method environmental protection simple for process,
Product adsorption capacity is superior.
Claims (8)
1. a kind of mask preparation method of graphene/active carbon in-situ plural gel adsorbent, which is characterized in that specific to prepare
Process is：
A. activated carbon is ground into 10 μm of powders below, is then dipped into alkaline reduction pore-creating liquid fully absorbing, so
After filter out material；
B. the activated carbon filtered out is scattered in graphene oxide solution, is then placed into the water heating kettle that can be turned upside down, water
It is rotated up and down in thermal process, cools down after completion of the reaction；
C. discharge water the graphene oxide/active carbon in-situ plural gel adsorbent heat-treated, is then cleaned with pure water, finally
It is dried to obtain final products.
2. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (a), ammonium hydroxide that the alkaline reduction pore-creating liquid of dipping is 15~20mol/L, sodium carbonate, potassium carbonate it is full
One or more of with aqueous solution, 10~60min of room temperature immersion time.
3. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (b), a concentration of 0.5~2g/L of graphene oxide, conductivity be less than 400 μ s/cm, graphene oxide with
Activated carbon dry ratio is 1:5~100.
4. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (b), water heating kettle be rotated up and down it is reverse, rotary speed be 10~60 minutes/circle.
5. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (b), 160 DEG C~250 DEG C of hydrothermal temperature, and hydro-thermal time 240min~600min.
6. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (c), the material that hydro-thermal finishes releasing is cleaned with pure water, and ejected wash water to conductance is less than 200 μ s/cm and stops
Cleaning.
7. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is, in step (c), the sample after cleaning uses vacuum drying or vacuum freezedrying.
8. the mask according to claim 1 preparation method of graphene/active carbon in-situ plural gel adsorbent, special
Sign is that the graphene in gel adsorber accounts for 1~5wt%, 900~1200m of specific surface area2/ g, mesoporous accounting 10~30%,
Micropore accounting 65~85%, remaining hole are macropore；Wherein, 0.35~2nm of radius is micropore, and radius is more than 2nm~50nm
Mesoporous, it is macropore that radius, which is more than 50nm,.
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Application publication date: 20181113 |