CN108043447A - A kind of photochemical catalyst preparation method and application - Google Patents
A kind of photochemical catalyst preparation method and application Download PDFInfo
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Classifications
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The present invention relates to field of waste water treatment, and in particular to a kind of photochemical catalyst preparation method and application.Include the following steps：Urea element calcining, obtains flaxen g C3N4；Gained g C3N4Bi (the NO being added to3)3Ethylene glycol solution in, stirred after first ultrasonic disperse, be added dropwise the ethylene glycol solution of KCl, completion of dropwise addition, stirring is stood again；Gained mixed solution centrifuges, and gives up supernatant, obtains sediment, then sediment washing, ethyl alcohol are washed；Drying, obtains g C3N4/ BiOCl laminated hetero knot photochemical catalysts.The g C that the present invention synthesizes3N4The photocatalysis sterilization function admirable of/BiOCl laminated hetero knot photochemical catalysts, synthetic method is simple, available for wastewater treatment, especially containing waste water such as Escherichia coli, pseudomonas aeruginosa, salmonella strains.
Description
Technical field
The present invention relates to field of waste water treatment, and in particular to a kind of photochemical catalyst preparation method and application.
Background technology
Drinking water safety is the significant problem for influencing national security, social stability and people's health.According to WHO group
The report knitted, due to not carrying out effective drinking water disinfection, the whole world has millions of people to die of water body carrying pathogen every year
Caused relevant disease, it is therefore desirable to which sterilization treatment is carried out to it.Currently used sterilization method has ultraviolet disinfection, ozone
Sterilizing, visible light catalytic sterilizing etc..Wherein, ultraviolet disinfection sterilizing and ozonization sterilizing can all generate health certain
Harm.And photocatalysis sterilization then has the characteristics that sterilizing efficiency height, nontoxic non-hazardous, non-secondary pollution, opens sterilizing field
New world.And developing a kind of high efficiency photocatalyst then becomes the core of photocatalysis sterilization technology.
Traditional photochemical catalyst is with TiO2Based on semiconductor.Prepare TiO2Method have very much, such as colloidal sol-solidifying
Glue method, hydro-thermal method, solvent-thermal method, direct oxidation method etc..As a kind of photochemical catalyst, TiO2Because having water insoluble, hydrophily,
Nontoxicity, cheap, biocompatibility, photochemical stability and suitably can band current potential the advantages that, be allowed to be widely used in light to urge
Change field.However, TiO2The shortcomings that also can not be ignored.In application process, there are sun light utilization efficiency is low, light induced electron is easily multiple for it
Conjunction leads to problems such as that quantum efficiency is low, back reaction easily carries out.Therefore, people are modified it.At present to TiO2Modified
Main means have noble metal loading, ion doping, ion implanting, semiconductors coupling, structural modification and dye sensitization etc..But
A kind of efficient, economic and that there is wide spectrum response photochemical catalyst could not be developed.
Graphite phase carbon nitride (g-C3N4) be used as a kind of 2D stratiforms nonmetallic materials, and with wider energy gap (~
2.7eV), the advantages that controllable band structure, synthetic method are simple, good thermal stability, be widely used in photocatalysis hydrogen production,
The processes such as organic matter degradation, carbon dioxide reduction, therefore cause the concern of vast researcher.At present, common g-C3N4
Synthetic method has thermal polymerization, solvent-thermal method, high temperature and high pressure method and sedimentation etc..But researchers are found in recent years,
Pure g-C3N4As semiconductor light-catalyst, since bandwidth is larger, photo-generated carrier is easily compound low with quantum efficiency etc. to ask
Topic, limits its application in environment and energy field.In order to improve g-C3N4Photocatalysis performance, researchers use
A variety of method of modifying, such as it is the doping of nonmetalloid, the doping of metallic element, codope, with other materials compound.But this
A little method manufacturing costs are high, and preparation condition is harsh, the preparation time cycle is long, is unfavorable for promoting and applying.Therefore, for g-C3N4Light
Catalyst preparation, how to overcome the shortcomings that preparation process is complicated, process conditions requirement is stringent, cost is higher is still that people face
Main problem.
The content of the invention
The technical problems to be solved by the invention are：There is provided that a kind of synthesis technology is simple, operating condition is mild, economical real
With the strong photochemical catalyst preparation method and application of, photo-catalysis capability.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of photochemical catalyst preparation method, including
Following steps：
Step 1, urea element calcine 2~3h under conditions of being placed in 500~600 DEG C, obtain flaxen g-C3N4；
Step 2, step 1 gained g-C3N4It is added to the Bi (NO of 0.01~0.02mol/L3)3Ethylene glycol solution in, first
15~30min of ultrasonic disperse stirs 10~20min, obtains g-C afterwards3N4With Bi (NO3)3The first mixed solution；
The ethylene glycol for the KCl that 0.01~0.02mol/L is added dropwise dropwise in first mixed solution obtained by step 3, step 2 is molten
Liquid after completion of dropwise addition, stirs 1~2h, then stands 2~4h and obtain the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 4~6min under the rotating speed of 8000~10000r/min, gives up
Supernatant obtains sediment, then the sediment is washed 1~3 time, and ethyl alcohol is washed 1~3 time；
Step 5, step 4 gained sediment are dried at 30~40 DEG C, and g-C is made3N4/ BiOCl laminated hetero knot photocatalysis
Agent.
Present invention additionally comprises g-C prepared by above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photochemical catalysts exist
Application in wastewater treatment.
The beneficial effects of the present invention are：Photochemical catalyst preparation method provided by the invention uses urea element to be closed for presoma
Stratiform bismuth oxychloride is synthesized in its surface in situ into graphite phase carbon nitride, and using coprecipitation, constructs graphite phase carbon nitride chlorine
Bismuth oxide stratiform hetero-junctions (g-C3N4/ BiOCl), g-C is obtained by the reaction using a series of3N4/ BiOCl laminated hetero knot light
Catalyst.
The g-C that the present invention synthesizes3N4The photocatalysis sterilization function admirable of/BiOCl laminated hetero knot photochemical catalysts, synthesis
Method is simple, available for wastewater treatment, especially containing waste water such as Escherichia coli, pseudomonas aeruginosa, salmonella strains.Simultaneously
It can avoid bringing chloroform etc. can be to the hurtful noxious material of health of human body as chlorination.The present invention adopts
Preparation method have simple process and low cost, preparation condition is mild, it is economical and practical the features such as, meet needs of production,
It can large-scale promotion use.
Description of the drawings
Fig. 1 is g-C prepared by the embodiment of the present invention 13N4/ BiOCl laminated hetero knot photochemical catalyst transmission electron microscope pictures；
Fig. 2 is g-C prepared by the embodiment of the present invention 13N4/ BiOCl laminated hetero knot photochemical catalysts and g-C3N4Laminated hetero
Tie the sterilization effect comparison diagram of photochemical catalyst；
Fig. 3 is g-C prepared by the embodiment of the present invention 23N4/ BiOCl laminated hetero knot photochemical catalysts and BiOCl laminated heteros
Tie the sterilization effect comparison diagram of photochemical catalyst；
Fig. 4 is g-C prepared by the embodiment of the present invention 33N4/ BiOCl laminated hetero knot photochemical catalysts and bulk-g-C3N4Light
The sterilization effect comparison diagram of catalyst；
Fig. 5 is g-C prepared by the embodiment of the present invention 13N4The XRD diagram of/BiOCl laminated hetero knot photochemical catalysts.
Specific embodiment
For the technology contents that the present invention will be described in detail, the objects and the effects, below in conjunction with embodiment and coordinate attached
Figure is explained.
The design of most critical of the present invention is:Urea element is used as precursor synthesis graphite phase carbon nitride, and using co-precipitation
Method synthesizes stratiform bismuth oxychloride, obtained g-C in graphite phase carbon nitride surface in situ3N4/ BiOCl laminated hetero knot photochemical catalysts
Photocatalysis sterilization function admirable.
A kind of photochemical catalyst preparation method, includes the following steps：
Step 1, urea element calcine 2~3h under conditions of being placed in 500~600 DEG C, obtain flaxen g-C3N4；
Step 2, step 1 gained g-C3N4It is added to the Bi (NO of 0.01~0.02mol/L3)3Ethylene glycol solution in, first
15~30min of ultrasonic disperse stirs 10~20min, obtains g-C afterwards3N4With Bi (NO3)3The first mixed solution；
The ethylene glycol for the KCl that 0.01~0.02mol/L is added dropwise dropwise in first mixed solution obtained by step 3, step 2 is molten
Liquid after completion of dropwise addition, stirs 1~2h, then stands 2~4h and obtain the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 4~6min under the rotating speed of 8000~10000r/min, gives up
Supernatant obtains sediment, then the sediment is washed 1~3 time, and ethyl alcohol is washed 1~3 time；
Step 5, step 4 gained sediment are dried at 30~40 DEG C, and g-C is made3N4/ BiOCl laminated hetero knot photocatalysis
Agent.
Further, the step 1 is specially：The urea element of 30~50g is weighed, is placed in 500~600 DEG C in Muffle furnace of item
2h is calcined under part, heating-up time 2h obtains flaxen g-C3N4。
Further, the step 2 is specially：Weigh 1.5~2g step 1 gained g-C3N4, it is added to 20~40mL's
Bi (the NO of 0.01~0.02mol/L3)3Ethylene glycol solution in, first 15~30min of ultrasonic disperse, afterwards stir 10~20min, obtain
To g-C3N4With Bi (NO3)3The first mixed solution.
Further, the step 4 is specially：Second mixed solution obtained by step 3 under the rotating speed of 10000r/min from
Heart 5min, gives up supernatant, obtains sediment, then the sediment is washed 2 times, and ethyl alcohol is washed 2 times.
Further, include the following steps：
Step 1, the urea element for weighing 30~50g are placed in Muffle furnace in crucible and calcine 2h under conditions of 550~600 DEG C,
Heating-up time is 2h, obtains flaxen g-C3N4；
Step 2 weighs 1.5~2g step 1 gained g-C3N4, the Bi of 0.01~0.02mol/L of 20~40mL of addition
(NO3)3Ethylene glycol solution in, first 15~30min of ultrasonic disperse, afterwards stir 10~20min, obtain g-C3N4With Bi (NO3)3's
First mixed solution；
It is added dropwise the KCl's of 0.01~0.02mol/L of 20~40mL in first mixed solution obtained by step 3, step 2 dropwise
Ethylene glycol solution after completion of dropwise addition, stirs 1~2h, then stands 2~4h and obtain the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, obtains
It is washed 2 times to sediment, then by the sediment, ethyl alcohol is washed 2 times；
Step 5, step 4 gained sediment are dried at 40 DEG C, and g-C is made3N4/ BiOCl laminated hetero knot photochemical catalysts.
Present invention additionally comprises g-C prepared by above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photochemical catalysts exist
Application in wastewater treatment.
Further, the water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, one kind of salmonella strain
It is or a variety of.
Embodiment 1
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 30g urea elements to be placed in crucible in Muffle furnace, and 2h is calcined at 550 DEG C, and temperature rises from room temperature
It is 2h to 550 DEG C of heating-up times, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 1.5g step 1 gained g-C3N4In beaker, 20mL0.01mol/LBi (NO are added in3)3Second two
Alcoholic solution after ultrasonic disperse 20min, in stirring 10min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing
Solution；
The ethylene glycol solution of the KCl of 20mL 0.01mol/L is added dropwise in first mixed solution obtained by step 3, step 2,
After the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 1h, stands 2h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, obtains
It is washed 2 times to sediment, then by the sediment, ethyl alcohol is washed 2 times；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 40 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
G-C made from embodiment 13N4The specific surface area of/BiOCl laminated hetero knot photochemical catalysts is 20m2/ g, Fig. 1 are this
G-C prepared by inventive embodiments 13N4/ BiOCl laminated hetero knot photochemical catalyst transmission electron microscope pictures, Fig. 5 make for the embodiment of the present invention 1
Standby g-C3N4The XRD diagram of/BiOCl laminated hetero knot photochemical catalysts.
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.
Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, the one or more of salmonella strain.
Comparative example 1
Comparative example 1 prepares g-C3N4In the step of/BiOCl laminated hetero knot photochemical catalysts, do not include the step 2 of embodiment 1
~step 5, i.e., do not load BiOCl, and other process conditions are same as Example 1.
G-C made from comparative example 13N4The specific surface area of laminated hetero knot photochemical catalyst is 99m2/g。
Photocatalysis sterilization aptitude tests are as follows：
This test experiments includes following four condition：Illumination adds in g-C made from embodiment 1 without catalyst, no light3N4/
BiOCl catalyst layers heterojunction photocatalyst, illumination add in g-C made from comparative example 13N4Laminated hetero knot photochemical catalyst, light
According to adding g-C made from the present embodiment 13N4/ BiOCl laminated hetero knot photochemical catalysts.
K12 strain Escherichia coli are put into and have been got ready in the conical flask equipped with nutrient broth, are vibrated under conditions of 37 DEG C
Cultivate 16h.After the completion of culture, removal nutrient solution aseptically is cleaned with physiological saline, then is diluted to original concentration.Then
Aseptically, drawing 8mL injections, sterilization is crossed in the reactor containing 72mL physiological saline, is placed in xenon lamp catalysis dress
In putting, 10~20min is stirred, coli somatic is made to be dispersed in physiological saline, by the physiology salt containing Escherichia coli
Water is placed in beaker.
0.1g catalyst accurately is weighed, is put into beaker, stirs 10~20min, after reacting 1h under the conditions of dark reaction, is opened
Xenon lamp is opened, carries out illumination, at interval of 1h 0.1mL mixed liquors is taken to dilute 105、106After times, draw 0.1mL dilutions and be uniformly applied to
On culture dish.After experiment, culture dish is put into 37 DEG C of constant incubator and cultivates 16h, then count Escherichia coli bacterium
Fall number, the results are shown in Figure 2.
This test experiments kills photocatalysis of the common e. coli k12 as subject evaluation synthetic catalyst using photocatalysis and goes out
Bacterium activity.As seen from Figure 2, when catalyst not illumination is added, the survival rate of bacterium is still more than 85%.It is being not added with being catalyzed
The trend that the survival rate of bacterium reduces under the direct illumination condition of agent is very slow, even across 7 illumination when small, still more than 80%
Above bacteria living illustrates that the efficiency of only illumination sterilization is very low.When under addition catalyst and illumination condition, it can be seen that
The survival rate of e. coli k12 is substantially reduced as the reaction time promotes, and illustrates that these materials all have photocatalysis sterilization activity,
But the catalytic activity of different materials has marked difference again.As the g-C of comparative example 13N4When making catalyst, Survival probability of bacteria is bright
Aobvious to decline, when 7 is small after light-catalyzed reaction, the Escherichia coli in water are not entirely killed, and still have 15% or so large intestine
Bacillus survives.And with g-C made from the present embodiment 13N4/ BiOCl for catalyst and add illumination when, photocatalysis sterilization activity significantly
It improves, bacterium can be killed when 6 is small or so, catalytic performance is significantly higher than other photochemical catalysts.
Embodiment 2
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 40g urea elements to be placed in crucible in Muffle furnace, and 2h is calcined at 550 DEG C, and temperature rises from room temperature
It is 2h to 550 DEG C of heating-up times, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 2g step 1 gained g-C3N4In beaker, 25mL 0.02mol/LBi (NO are added in3)3Ethylene glycol
Solution after ultrasonic disperse 20min, in stirring 10min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing it is molten
Liquid；
The ethylene glycol solution of the KCl of 25mL 0.02mol/L is added dropwise in first mixed solution obtained by step 3, step 2,
After the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 1h, stands 4h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, obtains
It is washed 2 times to sediment, then by the sediment, ethyl alcohol is washed 2 times；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 40 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
G-C made from embodiment 23N4The specific surface area of/BiOCl laminated hetero knot photochemical catalysts is 28.3m2/g。
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.
Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, the one or more of salmonella strain.
Comparative example 2
Comparative example 2 is not added with g-C3N4, prepare BiOCl：25mL 0.02mol/LBi(NO3)3Ethylene glycol solution solution in by
The ethylene glycol solution of the KCl of 25mL0.02mol/L is added dropwise to, after the ethylene glycol solution for dripping KCl, mixed solution continues to stir
After 1h, 4h is stood；Gained mixed solution centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, obtains sediment, then
The sediment is washed 2 times, ethyl alcohol is washed 2 times.
The specific surface area of BiOCl laminated heteros knot photochemical catalyst made from comparative example 2 is 3.3m2/g。
Photocatalysis sterilization aptitude tests are as follows：
This test experiments includes following four condition：Illumination adds in g- made from the present embodiment 2 without catalyst, no light
C3N4/ BiOCl laminated hetero knots photochemical catalyst, illumination add in BiOCl laminated hetero knots photochemical catalyst, illumination made from comparative example 2
Add g-C made from the present embodiment 23N4/ BiOCl laminated hetero knot photochemical catalysts.
K12 strain Escherichia coli are put into and have been got ready in the conical flask equipped with nutrient broth, are vibrated under conditions of 37 DEG C
Cultivate 16h.After the completion of culture, removal nutrient solution aseptically is cleaned with physiological saline, then is diluted to original concentration.Then
Aseptically, drawing 8mL injections, sterilization is crossed in the reactor containing 72mL physiological saline, is placed in xenon lamp catalysis dress
In putting, 10~20min is stirred, coli somatic is made to be dispersed in physiological saline, by the physiology salt containing Escherichia coli
Water is placed in beaker.
0.1g catalyst accurately is weighed, is put into above-mentioned beaker, 10~20min is stirred, 1h is reacted under the conditions of dark reaction
Afterwards, xenon lamp is opened, carries out illumination, at interval of 1h 0.1mL mixed liquors is taken to dilute 105、106After times, it is uniform to draw 0.1mL dilutions
It is applied on culture dish.After experiment, culture dish is put into 37 DEG C of constant incubator and cultivates 16h, then counts large intestine
Bacillus clump count records data, as a result such as Fig. 3.
As shown in figure 3, when catalyst not illumination is added and illumination is not added with catalyst, sterilization effect is the same as shown in Fig. 2.When
It adds under catalyst and illumination condition, it can be seen that the survival rate of e. coli k12 is substantially reduced as the reaction time promotes, and is said
These bright materials all have photocatalysis sterilization activity, but the catalytic activity of different materials has marked difference again.When BiOCl is done
During catalyst, Survival probability of bacteria is decreased obviously, but when 7 is small after light-catalyzed reaction, the Escherichia coli in water are not complete
It is complete to kill, still there is 20% or so Escherichia coli survival.And g-C is added with illumination3N4When/BiOCl is catalyst, photocatalysis sterilization
Activity significantly improves, and can kill bacterium when 6 is small or so, catalytic performance is significantly higher than BiOCl photochemical catalysts.
Embodiment 3
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 40g urea elements to be placed in crucible in Muffle furnace, and 2h is calcined at 550 DEG C, and temperature rises from room temperature
It is 2h to 550 DEG C of heating-up times, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 2g step 1 gained g-C3N4In beaker, 25mL 0.02mol/LBi (NO are added in3)3Ethylene glycol
Solution after ultrasonic disperse 20min, in stirring 10min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing it is molten
Liquid；
The ethylene glycol solution of the KCl of 25mL 0.02mol/L is added dropwise in first mixed solution obtained by step 3, step 2,
After the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 1h, stands 4h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, obtains
It is washed 2 times to sediment, then by the sediment, ethyl alcohol is washed 2 times；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 40 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
G-C made from embodiment 33N4The specific surface area of/BiOCl laminated hetero knot photochemical catalysts is 28.3m2/g。
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, salmonella
The one or more of kind.
Comparative example 3
Comparative example 3 prepares bulk-g-C3N4The step of photochemical catalyst, specific preparation method was：
10g melamines is taken to be placed in crucible in Muffle furnace, and are calcined at 520 DEG C, wherein being risen to from room temperature
520 DEG C of heating-up time is 2h, and calcination time 4h obtains faint yellow sample, is body phase graphite phase carbon nitride (bulk-g-
C3N4)；
Bulk-g-C made from comparative example 33N4The specific surface area of photochemical catalyst is 15.6m2/g。
Photocatalysis sterilization aptitude tests are as follows：
This test experiments includes following four condition：Illumination adds in g- made from the present embodiment 3 without catalyst, no light
C3N4/ BiOCl laminated hetero knots photochemical catalyst, illumination add in bulk-g-C made from comparative example 33N4Photochemical catalyst, illumination add this
G-C made from embodiment 33N4/ BiOCl laminated hetero knot photochemical catalysts.
K12 strain Escherichia coli are put into and have been got ready in the conical flask equipped with nutrient broth, are vibrated under conditions of 37 DEG C
Cultivate 16h.After the completion of culture, removal nutrient solution aseptically is cleaned with physiological saline, then is diluted to original concentration.Then
Aseptically, drawing 8mL injections, sterilization is crossed in the reactor containing 72mL physiological saline, is placed in xenon lamp catalysis dress
In putting, 10~20min is stirred, coli somatic is made to be dispersed in physiological saline, by the physiology salt containing Escherichia coli
Water is placed in beaker.
0.1g catalyst accurately is weighed, is put into above-mentioned beaker, 10~20min is stirred, 1h is reacted under the conditions of dark reaction
Afterwards, xenon lamp is opened, carries out illumination, at interval of 1h 0.1mL mixed liquors is taken to dilute 105、106After times, it is uniform to draw 0.1mL dilutions
It is applied on culture dish.After experiment, culture dish is put into 37 DEG C of constant incubator and cultivates 16h, then counts large intestine
Bacillus clump count records data, and the results are shown in Figure 4.
As shown in figure 4, when catalyst not illumination is added and illumination is not added with catalyst, the same Fig. 2 of sterilization effect.When
bulk-g-C3N4When making catalyst, Survival probability of bacteria is decreased obviously, but when 7 is small after light-catalyzed reaction, the large intestine in water
Bacillus is not entirely killed, and still has 40% or so Escherichia coli survival.And with g-C3N4/ BiOCl adds illumination for catalyst
When, photocatalysis sterilization activity significantly improves, and can kill bacterium when 5 is small or so, catalytic performance is significantly higher than bulk-g-
C3N4Photochemical catalyst.
Embodiment 4
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 40g urea elements to be placed in crucible in Muffle furnace, and 3h is calcined at 500 DEG C, and temperature rises from room temperature
It is 2h to 500 DEG C of heating-up times, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 1.8g step 1 gained g-C3N4In beaker, 20mL0.02mol/LBi (NO are added in3)3Second two
Alcoholic solution after ultrasonic disperse 15min, in stirring 10min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing
Solution；
The ethylene glycol solution of the KCl of 20mL 0.02mol/L is added dropwise in first mixed solution obtained by step 3, step 2,
After the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 1h, stands 2h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 6min under the rotating speed of 8000r/min, gives up supernatant, obtains
It is washed 1 time to sediment, then by the sediment, ethyl alcohol is washed 1 time；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 30 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, salmonella
The one or more of kind.
Embodiment 5
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 40g urea elements to be placed in crucible in Muffle furnace, and 2.5h is calcined at 550 DEG C, and temperature rises from room temperature
It is 2h to 550 DEG C of heating-up times, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 1.8g step 1 gained g-C3N4In beaker, 30mL0.015mol/LBi (NO are added in3)3Second two
Alcoholic solution after ultrasonic disperse 20min, in stirring 15min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing
Solution；
The ethylene glycol for the KCl that 30mL 0.015mol/L are added dropwise in first mixed solution obtained by step 3, step 2 is molten
Liquid, after the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 1.5h, stands 3h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 9000r/min, gives up supernatant, obtains
It is washed 2 times to sediment, then by the sediment, ethyl alcohol is washed 2 times；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 35 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, salmonella
The one or more of kind.
Embodiment 6
A kind of g-C3N4The preparation method of/BiOCl laminated hetero knot photochemical catalysts, comprises the following steps：
Step 1 takes 50g urea elements to be placed in crucible in Muffle furnace, and calcines 2h at 600 DEG C, and temperature rises to from room temperature
600 DEG C of heating-up time is 2h, obtains faint yellow sample, is thin layer graphite phase carbon nitride (g-C3N4)；
Step 2 weighs 2g step 1 gained g-C3N4In beaker, 40mL 0.01mol/LBi (NO are added in3)3Ethylene glycol
Solution after ultrasonic disperse 30min, in stirring 20min on magnetic stirring apparatus, obtains g-C3N4With Bi (NO3)3First mixing it is molten
Liquid；
The ethylene glycol solution of the KCl of 40mL 0.01mol/L is added dropwise in first mixed solution obtained by step 3, step 2,
After the ethylene glycol solution for dripping KCl, mixed solution continues after stirring 2h, stands 4h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 4min under the rotating speed of 10000r/min, gives up supernatant, obtains
It is washed 3 times to sediment, then by the sediment, ethyl alcohol is washed 3 times；
G-C is made in step 5, step 4 the gained sediment vacuumizing and drying at 40 DEG C3N4/ BiOCl laminated hetero knot light is urged
Agent.
The present invention also provides g-C prepared by a kind of above-mentioned photochemical catalyst preparation method3N4/ BiOCl laminated hetero knot photocatalysis
The application of agent, applied to wastewater treatment.Water in the wastewater treatment contains Escherichia coli, pseudomonas aeruginosa, salmonella
The one or more of kind.
In conclusion photochemical catalyst preparation method provided by the invention, uses urea element to be nitrogenized for precursor synthesis graphite-phase
Carbon, and stratiform bismuth oxychloride is synthesized in its surface in situ using coprecipitation, it is different to construct graphite phase carbon nitride bismuth oxychloride stratiform
Matter knot (g-C3N4/ BiOCl), g-C is obtained by the reaction using a series of3N4/ BiOCl laminated hetero knot photochemical catalysts.
The g-C that the present invention synthesizes3N4The photocatalysis sterilization function admirable of/BiOCl laminated hetero knot photochemical catalysts, synthesis
Method is simple, available for wastewater treatment, especially containing waste water such as Escherichia coli, pseudomonas aeruginosa, salmonella strains.Simultaneously
It can avoid bringing chloroform etc. can be to the hurtful noxious material of health of human body as chlorination.The present invention adopts
Preparation method have simple process and low cost, preparation condition is mild, it is economical and practical the features such as, meet needs of production,
It can large-scale promotion use.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalents that bright specification and accompanying drawing content are made directly or indirectly are used in relevant technical field, similarly include
In the scope of patent protection of the present invention.
Claims (7)
1. a kind of photochemical catalyst preparation method, which is characterized in that include the following steps：
Step 1, urea element calcine 2~3h under conditions of being placed in 500~600 DEG C, obtain flaxen g-C3N4；
Step 2, step 1 gained g-C3N4It is added to the Bi (NO of 0.01~0.02mol/L3)3Ethylene glycol solution in, ultrasonic disperse
15~30min stirs 10~20min, obtains g-C3N4With Bi (NO3)3The first mixed solution；
The ethylene glycol solution of the KCl of 0.01~0.02mol/L, drop is added dropwise in first mixed solution obtained by step 3, step 2 dropwise
After adding, 1~2h is stirred, then stands 2~4h and obtains the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 4~6min under the rotating speed of 8000~10000r/min, gives up supernatant
Liquid obtains sediment, then the sediment is washed 1~3 time, and ethyl alcohol is washed 1~3 time；
Step 5, step 4 gained sediment are dried at 30~40 DEG C, and g-C is made3N4/ BiOCl laminated hetero knot photochemical catalysts.
2. photochemical catalyst preparation method according to claim 1, which is characterized in that the step 1 is specially：Weigh 30~
The urea element of 50g, is placed in Muffle furnace and 2h is calcined under conditions of 500~600 DEG C, heating-up time 2h obtains flaxen g-
C3N4。
3. photochemical catalyst preparation method according to claim 1, which is characterized in that the step 2 is specially：Weigh 1.5
~2g step 1 gained g-C3N4, it is added to the Bi (NO of 0.01~0.02mol/L of 20~40mL3)3Ethylene glycol solution in, first
15~30min of ultrasonic disperse stirs 10~20min, obtains g-C afterwards3N4With Bi (NO3)3The first mixed solution.
4. photochemical catalyst preparation method according to claim 1, which is characterized in that the step 4 is specially：Step 3 institute
The second mixed solution centrifuges 5min under the rotating speed of 10000r/min, give up supernatant, obtain sediment, then by the precipitation
Object is washed 2 times, and ethyl alcohol is washed 2 times.
5. photochemical catalyst preparation method according to claim 1, which is characterized in that include the following steps：
Step 1, the urea element for weighing 30~50g are placed in Muffle furnace in crucible and calcine 2h under conditions of 550~600 DEG C, heating
Time is 2h, obtains flaxen g-C3N4；
Step 2 weighs 1.5~2g step 1 gained g-C3N4, the Bi (NO of 0.01~0.02mol/L of 20~40mL of addition3)3's
In ethylene glycol solution, first 15~30min of ultrasonic disperse stirs 10~20min, obtains g-C afterwards3N4With Bi (NO3)3It is first mixed
Close solution；
The second two of the KCl of 0.01~0.02mol/L of 20~40mL is added dropwise in first mixed solution obtained by step 3, step 2 dropwise
Alcoholic solution after completion of dropwise addition, stirs 1~2h, then stands 2~4h and obtain the second mixed solution；
Second mixed solution obtained by step 4, step 3 centrifuges 5min under the rotating speed of 10000r/min, gives up supernatant, is sunk
Starch, then the sediment is washed 2 times, ethyl alcohol is washed 2 times；
Step 5, step 4 gained sediment are dried at 40 DEG C, and g-C is made3N4/ BiOCl laminated hetero knot photochemical catalysts.
6. the g-C prepared according to any photochemical catalyst preparation method of Claims 1 to 53N4/ BiOCl laminated hetero knot light
The application of catalyst in the treatment of waste water.
7. the application of photochemical catalyst according to claim 6, which is characterized in that the water in the wastewater treatment contains large intestine
Bacillus, pseudomonas aeruginosa, the one or more of salmonella strain.
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| CN115501893A (en) * | 2022-09-29 | 2022-12-23 | 塔里木大学 | Novel g-C 3 N 5 Preparation method of-BiOCl heterojunction photocatalyst |
| CN115999603A (en) * | 2022-11-30 | 2023-04-25 | 莆田学院 | Method for constructing graphite phase carbon nitride/bismuth tungstate nano heterojunction |
| CN116371447A (en) * | 2023-04-21 | 2023-07-04 | 上海电力大学 | double-Z heterojunction photocatalyst and preparation method and application thereof |
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