CN107812509A - A kind of filter membrane material and its preparation method and application - Google Patents
A kind of filter membrane material and its preparation method and application Download PDFInfo
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- CN107812509A CN107812509A CN201710828587.9A CN201710828587A CN107812509A CN 107812509 A CN107812509 A CN 107812509A CN 201710828587 A CN201710828587 A CN 201710828587A CN 107812509 A CN107812509 A CN 107812509A
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- filter membrane
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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
-
- 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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention relates to the present invention relates to filtering material technical field, a kind of preparation method of filter membrane material is disclosed, this method includes：Transition metal salt is dissolved in solvent, after forming solution, carbon film is added, after being well mixed, is added in autoclave and is reacted, after being evacuated in autoclave, be filled with CO2It is 80 ~ 150bar to its internal absolute pressure, is warming up to 35 ~ 60oC, start to react, after reacting 0.5 ~ 24h, discharge CO2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid, dried, obtain presoma carbon film, under protective gas atmosphere, the presoma carbon film is reacted into 2 ~ 8h under the conditions of 700 ~ 1000 DEG C, obtains transition metal/carbon composite membrane, is immersed in the CS of sulphur2In solution, after soaking 1 ~ 12h, filter, dry, produce filter membrane material；The filter membrane material prepared by the present invention, transition metal Load Balanced, uniformity is good, has the characteristics that high adsorption efficiency and high-adsorption-capacity, and filter membrane material is separated from water easily, and recovery is simple, suitable for industrialized production.
Description
Technical field
The present invention relates to filtering material technical field, more particularly to a kind of filter membrane material and its preparation method and application.
Background technology
China's total mercury consumption figure about at 1000 tons or so, accounts for the 50% of world's aggregate consumption, is global maximum consumption
State and producing country.It however, mercury has the neurotoxicity of height, can enter by all means in organism, and be difficult to be metabolized, because
This causes cumulative effect in vivo, and grave danger is formed to human health.Therefore, the preventing and treating for mercury pollution is carved and not allowed
It is slow.
So far, the treatment technology of mercury-containing waste water mainly has chemical method, electrolysis, ion-exchange and absorption method etc..Wherein
Absorption method is technological means most commonly seen in demercuration technology.Demercuration adsorbent mainly includes carbon-supported catalyst, oxide-base is inhaled
Attached dose, ore class adsorbent and noble metal base adsorbent etc..From the point of view of actual demercuration effect, carbon-supported catalyst has hair because of it
Pore structure, huge surface area and the abundant surface functional group reached, is most ripe, efficient, cheap demercuration adsorbent.But
It is that the undressed carbon-supported catalyst overwhelming majority belongs to physical absorption, the active sites for the mercury that can be provided are less, cause its demercuration
It is less efficient.Therefore, the problem of adsorbent removed currently used for mercury ion in water is primarily present following several respects：（1）Absorption
Agent finite capacity；（2）Poor selectivity；（3）Adsorbent is mostly powder, is not readily separated with water, and recovery is difficult.Therefore, exploitation absorption
Capacity reaches, and selectivity is high, and the high-efficiency adsorbent easily reclaimed is very necessary.
The content of the invention
To solve the above problems, the present invention provides a kind of filter membrane material and preparation method thereof.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of preparation method of filter membrane material, it is characterised in that this method comprises the following steps：
（1）Transition metal salt is dissolved in solvent, solution is formed after being uniformly dissolved；
（2）To step（1）Carbon film is added in obtained 10-60ml solution, after being well mixed, is added to 100ml autoclaves
In reacted, be 0.01 ~ 0.1MPa by autoclave degree of being evacuated, be filled with CO2Absolute pressure is 8 inside to autoclave
~ 15MPa, is warming up to 35 ~ 60oC, start to react, after reacting 0.5 ~ 24h, discharge the CO in autoclave2To normal pressure, and cool down
To room temperature, reaction kettle liquid is obtained；
（3）Reaction kettle liquid is evaporated, solvent evaporated, remaining solids is dried, and obtains presoma carbon film；
（4）Under protective gas atmosphere, 2 ~ 8h is reacted under the conditions of being 700 ~ 1000 DEG C in reaction temperature by the presoma carbon film,
Obtain transition metal/carbon composite membrane；
（5）The transition metal/carbon composite membrane is immersed in the CS of 10ml sulphur2In solution, after soaking 1 ~ 12h, filter, dry,
Produce filter membrane material.
Preferably, the transition metal salt is one in iron, cobalt, nickel, manganese, copper, the sulfate of zinc, nitrate or villaumite
Kind is a variety of, and transition metal salt is turned into transition metal simple substance by above-mentioned preparation method step, has stronger reproducibility, can
Mercury ion is reduced into mercury simple substance.
Preferably, the solvent is at least one of water, ethanol, isopropanol, solvent can dissolve transition gold well
Belong to salt, form uniform solution, transition metal salt can hydrolyze in a solvent.
Preferably, the step（1）In, the molar concentration of transition metal salt is 0.01 ~ 1mol/L in solution.
Preferably, the step（2）In, carbon film is at least one of carbon paper, carbon cloth, carbon fiber, and it adds quality
For 0.5 ~ 10g, carbon film is several millimeters to several centimetres of size, can be bulk or sheet, can be rendered as spherical, rectangle, circle,
The shapes such as irregular polygon, carbon film provide avtive spot as carrier for transition metal simple substance and sulphur simple substance.
Preferably, the step（4）In, protective gas Ar, H2、N2At least one of, the mistake in presoma carbon film
Cross metal in the form of hydroxide to exist, under the high temperature conditions, it is carried out by carbon film to be reduced into transition metal simple substance, protect
Gas is to prevent the transition metal simple substance after reduction to be oxidized.
Preferably, the step（4）In, the reaction temperature is preferably 750 ~ 900oC, the reaction time be preferably for 2 ~
4h。
Preferably, the step（5）In, the CS of sulphur2In solution, sulphur and CS2Mass volume ratio be 1 ~ 50：100g/
ML, sulphur possess the effect of Adsorption of Mercury simple substance.
Present invention also offers filter membrane material prepared by the above method.
Present invention also offers the application of above-mentioned filter membrane material mercury ion in liquid is removed.
When autoclave of the present invention is reacted, CO2Effect be to provide a kind of medium of supercriticality, face super
Under boundary's state, transition metal salt solution contacts more preferably harmonious with carbon film.
The present invention useful effect be：（1）The present invention utilizes transition metal by the carrying transition metal simple substance on carbon film
Strong reducing property, reduce mercury ion, the mercury ion in the aqueous solution is fixed on carbon film by then the chemisorbed by sulphur, so as to
The purification of Mercury sewage is realized, the filter membrane material has excellent mercury ion absorption property, choosing of the material to removal mercury ion
Selecting property is high, can be widely used for mercury ion field of waste water treatment；（2）The filter membrane material of gained, transition metal Load Balanced, unanimously
Good, the increase mercury adsorption site of controllability in filter membrane material of property, has high adsorption efficiency and high-adsorption-capacity；（3）Filtering
Membrane material is separated from water easily, and recovery is simple.
Brief description of the drawings
Accompanying drawing is for providing a further understanding of the present invention, and a part for constitution instruction, with following tool
Body implementation is used for explaining the present invention together, but is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the XRD photos of product obtained by embodiment 1.
Fig. 2 is the Adsorption of Mercury capacity curve of product obtained by embodiment 1.
Fig. 3 is the XRD photos of product obtained by embodiment 2.
Embodiment
Below by specific embodiment, and with reference to accompanying drawing, technical scheme is described in further detail.
Embodiment 1
Took 0.98g NiCl2·6H2O, it is dissolved in 30ml absolute ethyl alcohols, solution is formed after being uniformly dissolved, is added in above-mentioned solution
Enter 3g carbon cloths, after being well mixed, be put into 100mL autoclave and reacted in the lump.Treat that autoclave is evacuated
Spend after 0.1MPa, to be filled with CO2Gas, absolute pressure inside autoclave is reached 9 MPa, reacted under 40 DEG C of temperature conditionss
After 0.5 h, the CO in autoclave is discharged2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid；The reaction kettle liquid is existed
Solvent is volatilized under vacuum, after remaining solid is dried, is placed under argon gas protective gas atmosphere, with 5 DEG C/min liter
Warm speed rises to 800 DEG C, calcination time 2h, nickel carbon composite film material is obtained after cooling.Weigh 0.3g sulphur and be dissolved in the sulphur of 10ml bis-
Change in carbon, form the carbon disulfide solution of sulphur, above-mentioned nickel carbon composite film material is immersed in the carbon disulfide solution of above-mentioned sulphur
In, after soaking 6h, carbon disulfide is evaporated, dries, that is, obtains filter membrane material, its XRD spectrum is shown in Fig. 1.
With the filter membrane material of the gained of embodiment 1 mercury adsorption experiment is carried out by following conditions：With HgCl2For mercury source, configuration
Ion concentration of mercury is 50mg L-1Mercury solution 20ml as simulation Mercury sewage.
Mercury adsorption experiment is carried out with obtained filter membrane material, test condition is, at normal temperatures by obtained filter membrane
Material is immersed in configured Mercury sewage solution, and sorbing material adsorption efficiency of mercury ion in 5min reaches 83%,
The adsorption efficiency of mercury ion reaches 98% after 30min, and the Adsorption of Mercury capacity curve of filter membrane material is shown in Fig. 2.
Embodiment 2
Took 0.02g NiCl2·6H2O, it is dissolved in 10ml water, solution is formed after being uniformly dissolved, is added in above-mentioned solution
0.5g carbon papers, after being well mixed, it is put into 100mL autoclave and is reacted in the lump, treat that autoclave is evacuated
Spend after -0.05MPa, to be filled with CO2Gas, and autoclave inner absolute pressure is reached 8 MPa, in 60 DEG C of temperature conditionss
After 24 h of lower reaction, the CO in autoclave is discharged2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid；By the reactor
After liquid is fully dried, it is placed under argon gas protective gas atmosphere and rises to 900 DEG C with 5 DEG C/min heating rate, calcination time
3h, nickel carbon composite film material is obtained after cooling.Weigh 0.1g sulphur to be dissolved in 10ml carbon disulfide, the carbon disulfide for forming sulphur is molten
Liquid, above-mentioned nickel carbon composite film material is immersed in the carbon disulfide solution of above-mentioned sulphur, after soaking 1h, carbon disulfide evaporated,
Dry, that is, obtain filter membrane material, its XRD spectrum is shown in Fig. 3.
Mercury adsorption experiment is carried out with obtained filter membrane material, test condition is, at normal temperatures by obtained filter membrane
Material is immersed in configured Mercury sewage solution, and sorbing material adsorption efficiency of mercury ion in 5min reaches 80%,
Mercury ion adsorption efficiency reaches 97% after 40min.
Embodiment 3
Took 6.48g FeCl3, it is dissolved in 40ml absolute ethyl alcohols, solution is formed after being uniformly dissolved, 10g is added in above-mentioned solution
Carbon fiber, after being well mixed, add in 100mL autoclave and reacted together, treat autoclave degree of being evacuated
After 0.1MPa, CO is filled with2Gas, and the absolute pressure inside autoclave is reached 15 MPa, in 50 DEG C of temperature conditionss
After lower reaction 6h, the CO in autoclave is discharged2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid；By the reaction kettle liquid
After fully drying, it is placed under argon gas protective gas atmosphere and rises to 1000 DEG C with 5 DEG C/min heating rate, calcination time
4h, iron/carbon composite film material is obtained after cooling.Weigh 5g sulphur to be dissolved in 10ml carbon disulfide, form the carbon disulfide solution of sulphur,
Iron/carbon composite film material is immersed in the carbon disulfide solution of above-mentioned sulphur, after soaking 8h, carbon disulfide volatilized, is dried,
Obtain filter membrane material.
Mercury adsorption experiment is carried out with obtained filter membrane material, test condition is, at normal temperatures by obtained filter membrane
Material is immersed in configured Mercury sewage solution, and sorbing material adsorption efficiency of mercury ion in 3min reaches 90%,
Mercury ion adsorption efficiency reaches 99% after 20min.
Embodiment 4
Took 3.25g Fe (NO3)3·9H2O, it is dissolved in 35ml water, solution is formed after being uniformly dissolved, is added in above-mentioned solution
2.5g carbon fibers, after being well mixed, it is put into 100mL autoclave and is reacted in the lump, treat that autoclave is pumped into very
After reciprocal of duty cycle is 0.01MPa, CO is filled with2Gas, the absolute pressure inside autoclave is set to reach 10 MPa.In 35 DEG C of temperature strips
After reacting 12h under part, the CO in autoclave is discharged2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid；By the reaction
After kettle liquid is fully dried, it is placed under nitrogen protective gas atmosphere and rises to 750 DEG C with 5 DEG C/min heating rate, during calcining
Between 8h, iron/carbon composite film material is obtained after cooling.Weigh 2.0g sulphur to be dissolved in 10ml carbon disulfide, form the carbon disulfide of sulphur
Solution, iron/carbon composite film material is immersed in the carbon disulfide solution of above-mentioned sulphur, after soaking 12h, carbon disulfide volatilized,
Dry, that is, obtain filter membrane material.
Mercury adsorption experiment is carried out with obtained filter membrane material, test condition is, at normal temperatures by obtained filter membrane
Material is immersed in configured Mercury sewage solution, and sorbing material adsorption efficiency of mercury ion in 3min reaches 92%,
Mercury ion adsorption efficiency reaches 99% after 15min.
Embodiment described above is a kind of preferable scheme of the present invention, not the present invention is made any formal
Limitation, there are other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (10)
1. a kind of preparation method of filter membrane material, it is characterised in that this method comprises the following steps：（1）By transition metal salt
It is dissolved in solvent, solution is formed after being uniformly dissolved；（2）Take step（1）Obtained solution 10-60ml, carbon film is added, be well mixed
Afterwards, it is added in 100ml autoclaves and is reacted, after being 0.01 ~ 0.1MPa by autoclave degree of being evacuated, is filled with
CO2Absolute pressure is 8 ~ 15MPa inside to autoclave, is warming up to 35 ~ 60oC, start to react, after reacting 0.5 ~ 24h, discharge high pressure
CO in reactor2To normal pressure, and room temperature is cooled to, obtains reaction kettle liquid；（3）Reaction kettle liquid is evaporated, solvent is evaporated
Fall, remaining solids is dried, and obtains presoma carbon film；（4）Under protective gas atmosphere, the presoma carbon film is existed
Reaction temperature reacts 2 ~ 8h under the conditions of being 700 ~ 1000 DEG C, obtains transition metal/carbon composite membrane；（5）By the transition metal/carbon
Composite membrane is immersed in the CS of 10ml sulphur2In solution, after soaking 1 ~ 12h, filter, dry, produce filter membrane material.
2. the preparation method of a kind of filter membrane material according to claim 1, it is characterised in that the transition metal salt is
One or more in iron, cobalt, nickel, manganese, copper, the sulfate of zinc, nitrate or villaumite.
3. the preparation method of a kind of filter membrane material according to claim 1, it is characterised in that the solvent is water, second
At least one of alcohol, isopropanol.
A kind of 4. preparation method of filter membrane material according to claim 1, it is characterised in that the step（1）In, it is molten
The molar concentration of transition metal salt is 0.01 ~ 1mol/L in liquid.
A kind of 5. preparation method of filter membrane material according to claim 1, it is characterised in that the step（2）In, carbon
Film is at least one of carbon paper, carbon cloth, carbon fiber, and the addition quality of carbon film is 0.5 ~ 10g.
A kind of 6. preparation method of filter membrane material according to claim 1, it is characterised in that the step（4）In, protect
It is Ar, H to protect gas2、N2At least one of.
A kind of 7. preparation method of filter membrane material according to claim 1, it is characterised in that the step（4）In, institute
It is preferably 750 ~ 900 to state reaction temperatureoC, reaction time are 2 ~ 5h.
A kind of 8. preparation method of filter membrane material according to claim 1, it is characterised in that the step（5）In, institute
State the CS of sulphur2In solution, sulphur and CS2Mass volume ratio be 1 ~ 50：100 g/mL.
9. as the filter membrane material obtained by claim 1-8 any one.
10. the filter membrane material described in claim 9 removes the application of mercury ion in a liquid.
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2017
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