CN109775798A - Water purification method integrating photocatalysis and membrane filtration - Google Patents

Water purification method integrating photocatalysis and membrane filtration Download PDF

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Publication number
CN109775798A
CN109775798A CN201711134152.0A CN201711134152A CN109775798A CN 109775798 A CN109775798 A CN 109775798A CN 201711134152 A CN201711134152 A CN 201711134152A CN 109775798 A CN109775798 A CN 109775798A
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carbon nitride
phase carbon
solid
crucible
graphite phase
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黄冠博
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Tianjin Miaoyu Technology Development Co ltd
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Tianjin Miaoyu Technology Development Co ltd
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Abstract

The invention discloses a water purification method integrating photocatalysis and membrane filtration, which comprises the following steps: the method comprises the following steps: putting the melamine solid into a covered crucible, putting the crucible into a muffle furnace, heating the crucible to a certain temperature in a static air atmosphere at a certain heating rate, maintaining the temperature for a certain time, and cooling the crucible to room temperature at a certain cooling rate. Taking out, grinding the solid by a mortar, and carrying out ultrasonic treatment; step two: modified graphite phase carbon nitride is loaded on the anodic alumina film by using a suction filtration method. The photocatalysis and filtration unit of the invention is composed of modified graphite-phase carbon nitride with selective permeability. The graphite phase carbon nitride allows water molecules to pass through unimpeded, while other contaminant molecules do not pass through or have significant penetration resistance. Meanwhile, under the irradiation of visible light, the graphite-phase carbon nitride can also catalyze the degradation reaction of organic pollutants, so that the sewage can be thoroughly treated in one unit.

Description

A kind of process for purifying water of integrated light catalytic and film filtering
Technical field
The present invention relates to clean water treatment technical field, the process for purifying water of especially a kind of integrated light catalytic and film filtering.
Background technique
Persistence organic pollutant (POP) includes certain dyestuffs, antibiotic, pesticide, Endocrine Disrupting Chemicals (hormone) etc., tool There is the harm such as certain chemical/biological stability, extended residual, bioaccumulation, high toxicity.Conventional treating method, such as Activated carbon adsorption etc., is only enriched with, and can not thoroughly be eliminated, and these pollutants are often in surface water with lower dense Degree occurs, therefore is badly in need of efficiently thorough disposition method.
Summary of the invention
In view of the above problems, the object of the present invention is to provide the water purification sides that a kind of integrated light catalytic and film filter Method.
The technical scheme is that the process for purifying water of a kind of integrated light catalytic and film filtering, includes the following steps:
Step 1: modified graphite phase carbon nitride
Melamine solid is placed in the crucible of capping, Muffle furnace is put into, with certain heating rate in still air It is heated to certain temperature in atmosphere, maintains certain time, is cooled to room temperature with certain rate of temperature fall.By solid mortar after taking-up It is finely ground, ultrasonic treatment;
Step 2: filter assemblies are prepared
Modified graphite phase carbon nitride is loaded on anodic oxidation aluminum-based film using suction method.
Further, the preferred oxygen doping graphite phase carbon nitride of the step 1 or sulfur doping graphite phase carbon nitride.
Further, the specific process parameter of the oxygen doping graphite phase carbon nitride are as follows: melamine solid is placed in and is added In the crucible of lid, it is put into Muffle furnace, with 1-5 DEG C of min-1Heating rate be heated to 450-650 DEG C in still air atmosphere, 2-10h is maintained, with 1-5 DEG C of min-1Rate of temperature fall be cooled to room temperature.It is after taking-up that solid mortar is finely ground, polytetrafluoro is added In ethylene hydrothermal reaction kettle, and add water at inner liner of reaction kettle 2/3rds, 120-200 DEG C of heating reaction, after take out it is solid Body is ultrasonically treated 1-3h, power 100-500w.
Further, the specific process parameter of the sulfur doping graphite phase carbon nitride are as follows: by 10%-90% (quality percentage Than) thiocarbamide and melamine solid be placed in the crucible of capping, Muffle furnace is put into, with 1-5 DEG C of min-1Heating rate exist It is heated to 450-650 DEG C in still air atmosphere, 2-10h is maintained, with 1-5 DEG C of min-1Rate of temperature fall be cooled to room temperature;It takes It is after out that solid mortar is finely ground, add deionized water and is ultrasonically treated 1-3h, power 100-500w.
Further, the specific process parameter of the step 2 are as follows: be placed in suction funnel for anodised aluminium as filter membrane In, the aqueous dispersions for the modified graphite phase carbon nitride being ultrasonically treated are poured into suction funnel, take out aluminium oxide after water is drained Basement membrane, which is placed in a vacuum drying oven, removes remaining moisture.
Compared with prior art, the beneficial effects of the present invention are:
(1) photocatalytic oxidation degradation is a kind of deep oxidation water treatment technology, can be pair by organic pollutant exhaustive oxidation Environmentally friendly carbon dioxide and water, therefore have a clear superiority.Photocatalysis Function Material is fixed on filter assemblies by the present invention On, it avoids Conventional catalytic and reacts subsequent required catalyst lock out operation, simple and effective.In addition, modified graphite phase carbon nitride Energy band visible light can be absorbed, therefore do not need the energy such as additional ultraviolet light, device is placed under sunlight irradiation can be into Row light-catalyzed reaction, economical and energy saving.
(2) photocatalysis of the invention and filter element are made of the modified graphite phase carbon nitride with selective penetrated property.Stone Black phase carbon nitride can permit that hydrone is without hindrance to be passed through, other contaminant molecules cannot by or penetration resistance it is very big.Meanwhile Under the irradiation of visible light, graphite phase carbon nitride can also be catalyzed the degradation reaction of organic pollutant, to may be implemented in a list Sewage is administered thoroughly in member.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated.
Embodiment 1: oxygen doping graphite phase carbon nitride
Step 1: melamine solid being placed in the crucible of capping, Muffle furnace is put into, with 1 DEG C of min-1Heating speed Rate is heated to 450 DEG C in still air atmosphere, 10h is maintained, with 1 DEG C of min-1Rate of temperature fall be cooled to room temperature.After taking-up Solid mortar is finely ground, it is added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, and add water at inner liner of reaction kettle 2/3rds, 200 DEG C heating reaction, after take out solid, be ultrasonically treated 3h, power 100w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Embodiment 2: sulfur doping graphite phase carbon nitride
Step 1:: the thiocarbamide of 10% (mass percent) and melamine solid are placed in the crucible of capping, horse is put into Not furnace, with 5 DEG C of min-1Heating rate be heated to 650 DEG C in still air atmosphere, 2h is maintained, with 5 DEG C of min-1Drop Warm rate is cooled to room temperature;It is after taking-up that solid mortar is finely ground, add deionized water and is ultrasonically treated 1h, power 500w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Embodiment 3: oxygen doping graphite phase carbon nitride
Step 1: melamine solid being placed in the crucible of capping, Muffle furnace is put into, with 5 DEG C of min-1Heating speed Rate is heated to 650 DEG C in still air atmosphere, 2h is maintained, with 5 DEG C of min-1Rate of temperature fall be cooled to room temperature.It will after taking-up Solid mortar is finely ground, is added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, and add water at inner liner of reaction kettle 2/3rds, 120 DEG C Heating reaction, after take out solid, be ultrasonically treated 1h, power 500w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Embodiment 4: sulfur doping graphite phase carbon nitride
Step 1:: the thiocarbamide of 90% (mass percent) and melamine solid are placed in the crucible of capping, horse is put into Not furnace, with 1 DEG C of min-1Heating rate be heated to 450 DEG C in still air atmosphere, 10h is maintained, with 1 DEG C of min-1's Rate of temperature fall is cooled to room temperature;It is after taking-up that solid mortar is finely ground, add deionized water and is ultrasonically treated 3h, power 100w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Embodiment 5: oxygen doping graphite phase carbon nitride
Step 1: melamine solid being placed in the crucible of capping, Muffle furnace is put into, with 3 DEG C of min-1Heating speed Rate is heated to 500 DEG C in still air atmosphere, 6h is maintained, with 2 DEG C of min-1Rate of temperature fall be cooled to room temperature.It will after taking-up Solid mortar is finely ground, is added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, and add water at inner liner of reaction kettle 2/3rds, 160 DEG C Heating reaction, after take out solid, be ultrasonically treated 2h, power 300w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Embodiment 6: sulfur doping graphite phase carbon nitride
Step 1:: the thiocarbamide of 60% (mass percent) and melamine solid are placed in the crucible of capping, horse is put into Not furnace, with 2 DEG C of min-1Heating rate be heated to 600 DEG C in still air atmosphere, 8h is maintained, with 4 DEG C of min-1Drop Warm rate is cooled to room temperature;It is after taking-up that solid mortar is finely ground, add deionized water and is ultrasonically treated 2h, power 300w.
Step 2: being placed in anodised aluminium as filter membrane in suction funnel, the modified graphite phase nitrogen that will be ultrasonically treated The aqueous dispersions for changing carbon pour into suction funnel, and it is remaining to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Moisture.
Taking the above-mentioned ideal embodiment according to the present invention as inspiration, through the above description, relevant staff is complete Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention Property range is not limited to the contents of the specification, it is necessary to which the technical scope thereof is determined according to the scope of the claim.

Claims (5)

1. the process for purifying water of a kind of integrated light catalytic and film filtering, which comprises the steps of:
Step 1: modified graphite phase carbon nitride
Melamine solid is placed in the crucible of capping, Muffle furnace is put into, with certain heating rate in still air atmosphere In be heated to certain temperature, maintain certain time, be cooled to room temperature with certain rate of temperature fall.Solid is ground with mortar after taking-up Carefully, it is ultrasonically treated;
Step 2: filter assemblies are prepared
Modified graphite phase carbon nitride is loaded on anodic oxidation aluminum-based film using suction method.
2. the process for purifying water of a kind of integrated light catalytic according to claim 1 and film filtering, which is characterized in that the step One preferred oxygen doping graphite phase carbon nitride or sulfur doping graphite phase carbon nitride.
3. the process for purifying water of a kind of integrated light catalytic according to claim 2 and film filtering, which is characterized in that the oxygen is mixed The specific process parameter of miscellaneous graphite phase carbon nitride are as follows: melamine solid is placed in the crucible of capping, is put into Muffle furnace, with 1- 5℃·min-1Heating rate be heated to 450-650 DEG C in still air atmosphere, 2-10h is maintained, with 1-5 DEG C of min-1's Rate of temperature fall is cooled to room temperature.It is after taking-up that solid mortar is finely ground, it is added in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, and add water to At inner liner of reaction kettle 2/3rds, 120-200 DEG C of heating reaction, after take out solid, be ultrasonically treated 1-3h, power 100- 500w。
4. the process for purifying water of a kind of integrated light catalytic according to claim 2 and film filtering, which is characterized in that the sulphur is mixed The specific process parameter of miscellaneous graphite phase carbon nitride are as follows: set the thiocarbamide of 10%-90% (mass percent) with melamine solid In the crucible of capping, it is put into Muffle furnace, with 1-5 DEG C of min-1Heating rate be heated to 450- in still air atmosphere 650 DEG C, 2-10h is maintained, with 1-5 DEG C of min-1Rate of temperature fall be cooled to room temperature;It is after taking-up that solid mortar is finely ground, add Ionized water is simultaneously ultrasonically treated 1-3h, power 100-500w.
5. the process for purifying water of a kind of integrated light catalytic according to claim 1 and film filtering, which is characterized in that the step Two specific process parameter are as follows: be placed in anodised aluminium as filter membrane in suction funnel, the modified graphite that will be ultrasonically treated The aqueous dispersions of phase carbon nitride pour into suction funnel, and it is surplus to be placed in a vacuum drying oven removing for taking-up aluminium oxide basement membrane after water is drained Remaining moisture.
CN201711134152.0A 2017-11-15 2017-11-15 Water purification method integrating photocatalysis and membrane filtration Pending CN109775798A (en)

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