CN108114973A - A kind of molybdenum disulfide photocatalytic degradation plate and preparation method for soil remediation - Google Patents
A kind of molybdenum disulfide photocatalytic degradation plate and preparation method for soil remediation Download PDFInfo
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- CN108114973A CN108114973A CN201711468596.8A CN201711468596A CN108114973A CN 108114973 A CN108114973 A CN 108114973A CN 201711468596 A CN201711468596 A CN 201711468596A CN 108114973 A CN108114973 A CN 108114973A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/02—Soil-conditioning materials or soil-stabilising materials containing inorganic compounds only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C2101/00—In situ
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
Abstract
The present invention relates to soil remediation fields, disclose a kind of molybdenum disulfide photocatalytic degradation plate and preparation method for soil remediation.Including following preparation process：（1）Ammonium heptamolybdate and sulphur powder are added in deionized water, sodium hypophosphite is added in after grinding, slurry is made, material component is：Ammonium heptamolybdate 32 ~ 40%, sulphur powder 15 ~ 18%, deionized water 38 ~ 51%, sodium hypophosphite 2 ~ 4%；（2）By slurry coated on substrate, heating carries out hydro-thermal reaction, and molybdenum disulfide film is obtained after irradiation is dry；（3）Laser welding is carried out to molybdenum disulfide film, it is strong bonded.Photocatalytic degradation plate produced by the present invention compares common photochemical catalyst, big with the contact area of soil, and light energy absorption rate is high, and photocatalysis efficiency and soil remediation effect are good, durability is good simultaneously, prepares simply, easy to use, cost is relatively low, environmentally safe, has wide application prospect.
Description
Technical field
The present invention relates to soil remediation field, provide a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation and
Preparation method.
Background technology
Soil Environmental Pollution is increasingly severe at present, pollutes the situation faced also very severe.Soil pollution can cause grain
The underproduction is eaten, pollutant load is exceeded in crop is detrimental to health, and the serious consequences such as pollutes the environment.Therefore, development warp
Ji and efficient soil restoring technology, the protection for ecological environment, the quality safety of agricultural product and holding for social economy
Supervention exhibition has great importance.The recovery technique of contaminated soil has very much, and physical chemistry reparation, micro- can be roughly divided by principle
Biological prosthetic and phytoremediation, wherein photocatalysis technology are a kind of emerging deep soil oxidation recovery techniques.
Photochemical catalytic oxidation refers to that under the conditions of certain wavelength light is shone the separation of photo-generated carrier occurs for semi-conducting material, so
Light induced electron and hole are being combined living radical of the generation with oxidisability or reproducibility, this activity with lewis' acid afterwards
Organic matter macromolecules degradation can be carbon dioxide or other small organic molecules and water by free radical, this during the reaction
Semi-conducting material i.e. photochemical catalyst do not change in itself.The research of photocatalysis field is from initial experiment in the world
Phenomenon is found, the applied basic research of catalysis material is progressively turned to by fundamental research；It is explored progressively by catalysis material
Turn to high-efficiency photocatalysis material System Design.On research means, have been able to disclose photocatalysis material from molecule, atomic level
Expect basic physical properties and structure-effect relation of catalysis material, light-catalyzed reaction process and reaction are studied from femtosecond time scale
Mechanism.Modern science computational methods including first principle and molecular dynamics simulation, gradually in catalysis material object
Property with light-catalyzed reaction mechanism study in terms of play an important role.Using semiconductor physics, material science and catalytic chemistry as base
The more complete photocatalysis theoretical system of plinth is tentatively established.
Soil photocatalytic degradation (photodissociation) technology is an emerging deep soil oxidation recovery technique, can be applied to pesticide
Wait the reparation of contaminated soils.This method includes photodissociation and photocatalytic degradation, is an emerging deep oxidation treatment technology.Photodissociation
Directly or indirectly two ways can be divided into, the former makes organic compound occur chemical bond rupture or structural rearrangement, the latter be then by
Other compounds absorb photon, and degradation reaction occurs for induction pollutant.The soil texture, grain size, iron oxide content, soil moisture,
Soil pH value and thickness of soil etc. have apparent influence to photochemical catalytic oxidation organic pollution：Highly porous pollutant in soil
Migration rate is fast, and clay content is lower, and photodissociation is faster；Naturally iron oxide plays organic matter photodissociation important regulating and controlling effect in soil；Have
Machine matter can be used as a kind of light stabilizer；Soil moisture can reconcile absorption band；Thickness of soil influences optical filtering rate and incident light rate.
In photocatalysis, it is important to which the application of catalyst, molybdenum disulfide are used as with class graphene layer structure, good optics
Performance and electron transport property, in photocatalytic degradation organic matter and field, molybdenum disulfide is developed rapidly.Photocatalysis technology
One of today's society hot research field is become for soil remediation.
Chinese invention patent application number 201310238190.6 discloses a kind of biomass carbon base soil-repairing agent, including light
Catalytic oxidant and carrier, photocatalyst are titanium dioxide, and carrier is biomass carbon.Preparation process is：A. raw material is crushed；
B. the preparation of biological material；C. the preparation of biomass carbon base soil-repairing agent.
Chinese invention patent application number 201510309549.3 discloses a kind of chlorinated aromatic organic material contaminated soil and repaiies
The photocatalysis treatment device of multiple leacheate.Photocatalysis treatment device includes pending leacheate and adds in mouth, the reaction of photocatalysis main body
Pond, graphene-titanium dioxide nanotube photocatalysis composite plate and reuse elution fluid outlet.The invention is with Sol-Gel-like method
Graphene-titanium dioxide nanotube photocatalysis composite plate is prepared, surface catalyst load characteristic is homogeneous, and absorptivity is high, catalysis
Agent is not easily to fall off.
According to above-mentioned, when photocatalysis technology is used for soil remediation in existing scheme, affected by environment, photochemical catalyst and soil
It is difficult to fully absorb light energy after contact, and it is limited with soil contact product, cause catalytic effect weak, while conventional powder
Shape photochemical catalyst is difficult to be directly realized by the degradation to harmful substance in soil, in consideration of it, the present invention proposes a kind of novelty
For the molybdenum disulfide photocatalytic degradation plate and preparation method of soil remediation, above-mentioned technical problem can be effectively solved.
The content of the invention
It is big due to there is absorption illumination difficulty when application at present is used for soil remediation compared with wide Photocatalyst, with soil
Earth contact area is small, and catalytic effect is weak, and conventional grained catalyst is difficult to realize the fully degraded to soil pollutant, and soil is repaiied
Multiple effect is undesirable, and process is complicated and slow, and rehabilitation cost is higher.
To solve the above problems, the present invention uses following technical scheme：
A kind of molybdenum disulfide photocatalytic degradation plate and preparation method for soil remediation, the molybdenum disulfide photocatalytic degradation plate
Preparation process be divided into three phases：（1）The preparation of slurry；（2）The preparation of molybdenum disulfide film；（3）Molybdenum disulfide film
Welding；
A kind of preparation method of molybdenum disulfide photocatalytic degradation plate for soil remediation, the detailed process of preparation are：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, makes film and high reflection glass
Glass substrate is strong bonded, forms photocatalytic degradation plate thin plate；By direct sunlight, the back side is anti-by glass substrate in layer of molybdenum-disulfide front
Light is penetrated, so as to improve photocatalysis efficiency.
Preferably, in the slurry, the total mass fraction of each component in terms of 100 parts, wherein：32 ~ 40 parts of ammonium heptamolybdate, sulphur
15 ~ 18 parts of powder, 38 ~ 51 parts of deionized water, 2 ~ 4 parts of sodium hypophosphite；
Preferably, the ball mill is one kind in total volume ball mill or annular gap-type ball mill；After the powder mull
Grain size is 20 ~ 100nm；
Preferably, the wet grinding is using zirconium oxide bead as grinding bead；The zirconium oxide bead is stablized using iridium stabilization or caesium；It is described
A diameter of 10 ~ 50 μm of zirconium oxide bead；
Preferably, the slurry coating thickness is 0.5 ~ 2mm；
Preferably, the hydrothermal temperature is 180 ~ 200 DEG C, and the time is 18 ~ 22h；
Preferably, infrared drying or microwave drying can be used in the irradiation drying, and moisture content should be down to less than 3%；
Preferably, the laser welding uses carbon dioxide continuous laser welding, and protective gas is one in nitrogen, argon gas or helium
Kind；
Preferably, the laser power be 5 ~ 20kW, power density 104~106W/cm2, speed of welding is 2 ~ 5cm/s；
A kind of molybdenum disulfide photocatalytic degradation plate for soil remediation being prepared by the above method.
Photocatalytic degradation plate prepared by the test present invention with soil contact product, absorptivity and catalysis efficiency, and with
Powdery single catalyst, composite catalyst compare, and method of the invention has apparent long-acting advantage, as shown in table 1.
Table 1：
| Performance indicator | The present invention | Powdery single catalyst | Composite catalyst |
| It is accumulated with soil contact（cm2/g） | 50~100 | 20~30 | 10~20 |
| Absorptivity（%） | 70~90 | 30~50 | 40~60 |
| Catalysis efficiency | It is high | It is low | It is relatively low |
The present invention provides a kind of molybdenum disulfide photocatalytic degradation plate and preparation method for soil remediation, with prior art phase
Than, protrude the characteristics of and excellent effect be：
1st, the method for proposing the molybdenum disulfide photocatalytic degradation plate that high reflecting glass is used to be prepared for substrate for soil remediation.
2nd, film is formed on high rear reflector plate by hydro-thermal reaction, and passing through laser welding makes catalytic film securely weld
It is connected on rear reflector plate, gained photocatalytic degradation plate durability is good, easy to use.
3rd, photocatalytic degradation plate prepared by the present invention increases effectively the contact area of molybdenum disulfide catalyst and soil, carries
High light energy absorption rate, and then significantly improve photocatalysis efficiency and soil remediation effect.
4th, preparation process of the invention is environmentally safe, while manufacturing cost is relatively low, before having wide application
Scape.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Scope be only limitted to following example.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is total volume ball mill；Average grain diameter is 80nm after powder mull；
Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using iridium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：36 parts of ammonium heptamolybdate, 16 parts of sulphur powder, deionized water 45
Part, 3 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 1.0mm；Hydrothermal temperature is 190 DEG C, time 20h；Irradiation is dry to use infrared drying,
Moisture content is 2.5%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is nitrogen；Laser power is 12kW, power density 105W/cm2, speed of welding 4cm/s.
Photocatalytic degradation plate made from embodiment 1, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Embodiment 2
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is annular gap-type ball mill；Average grain diameter is after powder mull
20nm；Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using caesium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：32 parts of ammonium heptamolybdate, 15 parts of sulphur powder, deionized water 51
Part, 2 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 0.5mm；Hydrothermal temperature is 180 DEG C, time 22h；Irradiation is dry using microwave drying, contains
Water rate is 2.8%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is argon gas；Laser power is 5kW, power density 104W/cm2, speed of welding 2cm/s.
Photocatalytic degradation plate made from embodiment 2, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Embodiment 3
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is total volume ball mill；Average grain diameter is 60nm after powder mull；
Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using iridium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：40 parts of ammonium heptamolybdate, 18 parts of sulphur powder, deionized water 38
Part, 4 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 2mm；Hydrothermal temperature is 200 DEG C, time 18h；Irradiation is dry using microwave drying, aqueous
Rate is 2.3%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is helium；Laser power is 20kW, power density 106W/cm2, speed of welding 5cm/s.
Photocatalytic degradation plate made from embodiment 3, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Embodiment 4
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is annular gap-type ball mill；Average grain diameter is after powder mull
80nm；Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using caesium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：34 parts of ammonium heptamolybdate, 16 parts of sulphur powder, deionized water 48
Part, 2 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 0.8mm；Hydrothermal temperature is 190 DEG C, time 21h；Irradiation is dry using microwave drying, contains
Water rate is 2.6%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is nitrogen；Laser power is 8kW, power density 104W/cm2, speed of welding 3cm/s.
Photocatalytic degradation plate made from embodiment 4, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Embodiment 5
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is total volume ball mill；Average grain diameter is 30nm after powder mull；
Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using iridium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：38 parts of ammonium heptamolybdate, 17 parts of sulphur powder, deionized water 41
Part, 4 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 1.5mm；Hydrothermal temperature is 195 DEG C, time 19h；Irradiation is dry to use infrared drying,
Moisture content is 2.6%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is argon gas；Laser power is 17kW, power density 106W/cm2, speed of welding 4cm/s.
Photocatalytic degradation plate made from embodiment 5, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Embodiment 6
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is annular gap-type ball mill；Average grain diameter is after powder mull
50nm；Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using caesium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：36 parts of ammonium heptamolybdate, 16 parts of sulphur powder, deionized water 45
Part, 3 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
Slurry coating thickness is 1.2mm；Hydrothermal temperature is 190 DEG C, time 19h；Irradiation is dry using microwave drying, contains
Water rate is 2.5%；
（3）The detailed process of the welding of molybdenum disulfide film is：
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, the molybdenum disulfide on thin plate
By direct sunlight, the back side is improved photocatalysis efficiency by glass substrate reflected light in layer front；Laser welding is connected using carbon dioxide
Continuous Laser Welding, protective gas is helium；Laser power is 12kW, power density 105W/cm2, speed of welding 4cm/s.
Photocatalytic degradation plate made from embodiment 6, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Comparative example 1
（1）The detailed process of the preparation of slurry is：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；Ball mill is annular gap-type ball mill；Average grain diameter is after powder mull
50nm；Wet grinding is using zirconium oxide bead as grinding bead；Zirconium oxide bead is stablized using caesium；
In slurry, the total mass fraction of each component in terms of 100 parts, wherein：36 parts of ammonium heptamolybdate, 16 parts of sulphur powder, deionized water 45
Part, 3 parts of sodium hypophosphite；
（2）The detailed process of the preparation of molybdenum disulfide film is：
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum degradation plate；
Slurry coating thickness is 1.2mm；Hydrothermal temperature is 190 DEG C, time 19h；Irradiation is dry using microwave drying, contains
Water rate is 2.5%.
Photocatalytic degradation plate made from comparative example 1, with soil contact product, absorptivity and catalysis efficiency such as 2 institute of table
Show.
Table 2：
| Performance indicator | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example 1 |
| It is accumulated with soil contact（cm2/g） | 78.5 | 86.8 | 88.4 | 79.5 | 93.2 | 86.5 | 50.6 |
| Absorptivity（%） | 80.5 | 84.3 | 79.6 | 88.5 | 84.2 | 80.4 | 60.5 |
| 90 days catalysis efficiency attenuation rates（%） | 5.8 | 6.6 | 4.8 | 5.2 | 6.8 | 7.0 | 38.6 |
Claims (9)
1. a kind of preparation method of molybdenum disulfide photocatalytic degradation plate for soil remediation, the detailed process of preparation are：
First ammonium heptamolybdate and sulphur powder are added in deionized water, is placed in carrying out wet grinding in ball mill, add a certain amount of
Sodium hypophosphite, stir evenly obtained slurry；
First using high reflecting glass as substrate, slurry obtained is evenly applied on substrate, then raises temperature, makes ammonium heptamolybdate
Hydro-thermal reaction occurs with sulphur powder, in substrate surface in-situ preparation molybdenum disulfide nano sheet, then using irradiation drying, curing is made
Molybdenum film；
In the presence of protective gas, molybdenum disulfide film is welded using laser scanner technique, makes film and high reflection glass
Glass substrate is strong bonded, forms photocatalytic degradation plate thin plate；By direct sunlight, the back side is anti-by glass substrate in layer of molybdenum-disulfide front
Light is penetrated, so as to improve photocatalysis efficiency.
2. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：In the slurry, the total mass fraction of each component in terms of 100 parts, wherein：32 ~ 40 parts of ammonium heptamolybdate, sulphur powder 15 ~ 18
Part, 38 ~ 51 parts of deionized water, 2 ~ 4 parts of sodium hypophosphite.
3. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The ball mill is one kind in total volume ball mill or annular gap-type ball mill；Grain size after the powder mull
For 20 ~ 100nm.
4. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The wet grinding is using zirconium oxide bead as grinding bead；The zirconium oxide bead is stablized using iridium stabilization or caesium；The oxidation
A diameter of 10 ~ 50 μm of zirconium pearl.
5. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The slurry coating thickness is 0.5 ~ 2mm.
6. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The hydrothermal temperature is 180 ~ 200 DEG C, and the time is 18 ~ 22h.
7. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The irradiation is dry using infrared drying or microwave drying, and moisture content should be down to less than 3%.
8. the preparation method of a kind of molybdenum disulfide photocatalytic degradation plate for soil remediation according to claim 1, special
Sign is：The laser welding uses carbon dioxide continuous laser welding, and protective gas is one kind in nitrogen, argon gas or helium；
The laser power be 5 ~ 20kW, power density 104~106W/cm2, speed of welding is 2 ~ 5cm/s.
9. a kind of molybdenum disulfide photocatalytic degradation for soil remediation that any one of claim 1-8 the method is prepared
Plate.
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| JP2001070802A (en) * | 1999-09-03 | 2001-03-21 | Toshiba Corp | Photocatalyst film and its production |
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| CN104961353A (en) * | 2015-06-24 | 2015-10-07 | 中国科学院上海光学精密机械研究所 | Method for preparing large-size layered orthorhombic MoS2 nano-film of asymmetric structure under hydrothermal condition |
| CN106381481A (en) * | 2016-09-18 | 2017-02-08 | 河南师范大学 | Preparation method of metal doping molybdenum disulfide thin film |
| CN106732669A (en) * | 2016-12-21 | 2017-05-31 | 北京化工大学 | A kind of MoS as photoelectrocatalysis liberation of hydrogen material2/In2S3Composite catalyst and preparation method thereof |
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| CN111530908A (en) * | 2020-05-09 | 2020-08-14 | 中国石油大学(华东) | Combined treatment method for petroleum-polluted soil |
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