CN109248678A - A kind of preparation method of lightweight bismuth tungstate scavenging material - Google Patents
A kind of preparation method of lightweight bismuth tungstate scavenging material Download PDFInfo
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- CN109248678A CN109248678A CN201811143889.3A CN201811143889A CN109248678A CN 109248678 A CN109248678 A CN 109248678A CN 201811143889 A CN201811143889 A CN 201811143889A CN 109248678 A CN109248678 A CN 109248678A
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- lightweight
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- hollow ceramic
- bismuth tungstate
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 29
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 29
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 230000002000 scavenging effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000000919 ceramic Substances 0.000 claims abstract description 29
- 239000004005 microsphere Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 230000004913 activation Effects 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001214 Polysorbate 60 Polymers 0.000 claims abstract description 7
- 229960003511 macrogol Drugs 0.000 claims abstract description 7
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims abstract description 3
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims abstract description 3
- 229940113124 polysorbate 60 Drugs 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000003995 emulsifying agent Substances 0.000 claims description 6
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims 2
- 229920001223 polyethylene glycol Polymers 0.000 claims 2
- 239000010865 sewage Substances 0.000 abstract description 11
- 238000000746 purification Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000013019 agitation Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000003911 water pollution Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000006835 compression Effects 0.000 description 8
- 238000007906 compression Methods 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000003213 activating effect Effects 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011796 hollow space material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- B01J35/39—
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
A kind of preparation method of lightweight bismuth tungstate scavenging material, belongs to water pollution field of purification materials, including following processing steps: hollow ceramic microspheres being handled through NaOH solution, and through filtering, drying and calcination, obtain activation hollow ceramic microspheres；Wolframic acid is dissolved in NaOH solution, adds five nitric hydrate bismuths, adjusts solution ph, polysorbate60 and Liquid Macrogol is added, carries out hydro-thermal overlay film on activation hollow ceramic microspheres, then through drying and calcination, obtain lightweight bismuth tungstate scavenging material.The density of such material is slightly above common sewage, and simultaneously fast purification organic pollutant can be sufficiently mixed with water.It can be quickly separated from water when stopping agitation, be suitable for continuous sewage treatment technology.
Description
Technical field
The invention belongs to water pollution field of purification materials, and in particular to a kind of preparation side of lightweight bismuth tungstate scavenging material
Method.
Background technique
Between this 50 years of photocatalysis pollution purification techniques development, in relation to this technology in theoretical and application aspect research one
It is directly the important hot content of environmental pollution field of purification.Even to this day, the theoretical research of photocatalysis technology is mature, institute face
The research hotspot faced is the practical application in various depollution of environment fields.In order to reach this purpose, needing to pay special attention to has
The research and development of the material of light catalytic purifying function especially make its not only photocatalytic activity with higher, additionally it is possible to meet a variety of
The particular/special requirement of the actual production link of form.The main problem to be faced in water treatment procedure is net to sewage
After change processing, cleaned water is separated with catalysis material, to carry out the processing of next batch sewage.At one section
Supported materials in time as research hotspot can solve this problem, however film-type loads catalysis material often not
With with the comparable purification activity of granular material, not only it is easy to be separated from water to need to provide, but also there is high light catalysis work
The new material of property.Low-density hollow material can solve this difficulty.Such material have with density similar in water, slight
It can be sufficiently mixed with sewage when stirring or aeration, so as to give full play to the activity of catalysis material；Meanwhile stopping
After stirring, this material and purified water energy reach quick separating, convenient for discharge water purification.Using such material, it is ensured that even
To the separating technology requirement of catalysis material and water during continuous processing sewage.
Summary of the invention
In view of the problems of the existing technology, the present invention is intended to provide a kind of preparation side of lightweight bismuth tungstate scavenging material
Method, the lightweight bismuth tungstate scavenging material can be quickly separated from water after the dirty water decontamination handles process, and it is continuous to be suitable for sewage
Treatment process.
The technical solution adopted by the present invention is that:
A kind of preparation method of lightweight bismuth tungstate scavenging material, including following processing steps:
Step 1: activation hollow ceramic microspheres.
(1) NaOH solution of 50g hollow ceramic microspheres and the 0.3mol/L of 500mL are mixed, is heated to 65 DEG C, herein
Temperature 2h obtains mixture A.
(2) mixture A is filtered, is 7 with deionized water repeated flushing to filtrate pH value, obtains solids A.
(3) it by solids A in 110 DEG C of dry 10h, then in 800 DEG C of calcining 3h, is cooled to room temperature, obtains activating hollow pottery
Porcelain microballon.
Step 2: hydro-thermal overlay film.
(1) 9 ~ 12g wolframic acid is dissolved in the NaOH solution of 0.5mol/L of 300mL, adds 10 ~ 15g five and is hydrated nitre
Sour bismuth, stirring to formation solution A.
(2) under stirring into solution A be added dropwise 0.5mol/L hydrochloric acid solution, adjust solution ph be 9, then plus
Enter 6 ~ 10mL emulsifier tween 60 and 5 ~ 8mL Liquid Macrogol, stirring to formation solution B.
(3) solution B and activation hollow ceramic microspheres are mixed, moves into stainless steel hydrothermal reaction kettle, it is anti-at 210 ~ 230 DEG C
20h is answered, cooled and filtered obtains solids B.
Step 3: heat treatment.
By solids B in 110 DEG C of dry 10h, then in 710 ~ 780 DEG C of calcining 3h, it is cooled to room temperature, obtains lightweight wolframic acid
Bismuth scavenging material.
A kind of preparation method of above-mentioned lightweight bismuth tungstate scavenging material, in which:
The hollow ceramic microspheres are white ball, 8 ~ 26 μm of partial size, 0.5 ~ 0.6g/cm of density3, compression strength 3.5 × 105~
4.0×105Pa, 150 ~ 180m of specific surface area2/g.For known product.
The technical characteristics of lightweight bismuth tungstate scavenging material prepared by the present invention are as follows: 10 ~ 30 μm of partial size, density 1.2 ~
1.3g/cm3, compression strength 3.3 × 105~3.8×105Pa, 220 ~ 300m of specific surface area2/ g, refractoriness is less than 800 DEG C.
The invention belongs to water pollution field of purification materials, including following processing steps: hollow ceramic microspheres are molten through NaOH
Liquid processing, and through filtering, drying and calcination, obtain activation hollow ceramic microspheres；Wolframic acid is dissolved in NaOH solution, adds five
Nitric hydrate bismuth adjusts solution ph, and polysorbate60 and Liquid Macrogol is added, and carries out hydro-thermal on activation hollow ceramic microspheres
Overlay film, then through drying and calcination, obtain lightweight bismuth tungstate scavenging material.The density of such material is slightly above common sewage, energy
Enough and water is sufficiently mixed and fast purification organic pollutant.It can be quickly separated from water when stopping agitation.
The advantage is that:
For hollow ceramic microspheres after NaOH solution activates, surface is easy to affine with bismuth tungstate, can be on hollow ceramic microspheres surface
Form fine and close bismuth tungstate film, and the activity of light catalytic purifying dirt organic pollutants with higher.Such novel-section
The density of material is slightly above common sewage, can be sufficiently mixed under mild agitation state with water, so as to fully absorb light source
Radiation, and the organic pollutant in purifying sewage quickly.When processing terminate and stops agitation, this material can quickly and moisture
From to be suitable for continuous sewage treatment technology.
Specific embodiment
Chemical raw material used in following embodiments is all pure material.
Embodiment 1
A kind of preparation method of lightweight bismuth tungstate scavenging material, including following processing steps:
Step 1: activation hollow ceramic microspheres.
(1) NaOH solution of 50g hollow ceramic microspheres and the 0.3mol/L of 500mL are mixed, is heated to 65 DEG C, herein
Temperature 2h obtains mixture A.
(2) mixture A is filtered, is 7 with deionized water repeated flushing to filtrate pH value, obtains solids A.
(3) it by solids A in 110 DEG C of dry 10h, then in 800 DEG C of calcining 3h, is cooled to room temperature, obtains activating hollow pottery
Porcelain microballon.
Step 2: hydro-thermal overlay film.
(1) 9g wolframic acid is dissolved in the NaOH solution of 0.5mol/L of 300mL, adds five nitric hydrate bismuth of 10g,
Stirring extremely forms solution A.
(2) under stirring into solution A be added dropwise 0.5mol/L hydrochloric acid solution, adjust solution ph be 9, then plus
Enter 6mL emulsifier tween 60 and 5mL Liquid Macrogol, stirring to formation solution B.
(3) solution B and activation hollow ceramic microspheres are mixed, moves into stainless steel hydrothermal reaction kettle, reacted at 210 DEG C
20h, cooled and filtered obtain solids B.
Step 3: heat treatment.
By solids B in 110 DEG C of dry 10h, then in 710 DEG C of calcining 3h, it is cooled to room temperature, it is net obtains lightweight bismuth tungstate
Change material.
The hollow ceramic microspheres are white ball, 8 μm of partial size, density 0.6g/cm3, compression strength 4 × 105Pa compares table
Area 180m2/g。
The technical characteristics of the lightweight bismuth tungstate scavenging material of preparation are as follows: 10 μm of partial size, density 1.3g/cm3, resistance to compression
Intensity 3.8 × 105Pa, specific surface area 300m2/ g, refractoriness is less than 800 DEG C.
Embodiment 2
A kind of preparation method of lightweight bismuth tungstate scavenging material, including following processing steps:
Step 1: activation hollow ceramic microspheres.
(1) NaOH solution of 50g hollow ceramic microspheres and the 0.3mol/L of 500mL are mixed, is heated to 65 DEG C, herein
Temperature 2h obtains mixture A.
(2) mixture A is filtered, is 7 with deionized water repeated flushing to filtrate pH value, obtains solids A.
(3) it by solids A in 110 DEG C of dry 10h, then in 800 DEG C of calcining 3h, is cooled to room temperature, obtains activating hollow pottery
Porcelain microballon.
Step 2: hydro-thermal overlay film.
(1) 10g wolframic acid is dissolved in the NaOH solution of 0.5mol/L of 300mL, adds five nitric hydrate bismuth of 12g,
Stirring extremely forms solution A.
(2) under stirring into solution A be added dropwise 0.5mol/L hydrochloric acid solution, adjust solution ph be 9, then plus
Enter 8mL emulsifier tween 60 and 6mL Liquid Macrogol, stirring to formation solution B.
(3) solution B and activation hollow ceramic microspheres are mixed, moves into stainless steel hydrothermal reaction kettle, reacted at 220 DEG C
20h, cooled and filtered obtain solids B.
Step 3: heat treatment.
By solids B in 110 DEG C of dry 10h, then in 750 DEG C of calcining 3h, it is cooled to room temperature, it is net obtains lightweight bismuth tungstate
Change material.
The hollow ceramic microspheres are white ball, 18 μm of partial size, density 0.5g/cm3, compression strength 3.8 × 105Pa, than
Surface area 170m2/g。
The technical characteristics of the lightweight bismuth tungstate scavenging material of preparation are as follows: 20 μm of partial size, density 1.2g/cm3, resistance to compression
Intensity 3.6 × 105Pa, specific surface area 260m2/ g, refractoriness is less than 800 DEG C.
Embodiment 3
A kind of preparation method of lightweight bismuth tungstate scavenging material, including following processing steps:
Step 1: activation hollow ceramic microspheres.
(1) NaOH solution of 50g hollow ceramic microspheres and the 0.3mol/L of 500mL are mixed, is heated to 65 DEG C, herein
Temperature 2h obtains mixture A.
(2) mixture A is filtered, is 7 with deionized water repeated flushing to filtrate pH value, obtains solids A.
(3) it by solids A in 110 DEG C of dry 10h, then in 800 DEG C of calcining 3h, is cooled to room temperature, obtains activating hollow pottery
Porcelain microballon.
Step 2: hydro-thermal overlay film.
(1) 12g wolframic acid is dissolved in the NaOH solution of 0.5mol/L of 300mL, adds five nitric hydrate bismuth of 15g,
Stirring extremely forms solution A.
(2) under stirring into solution A be added dropwise 0.5mol/L hydrochloric acid solution, adjust solution ph be 9, then plus
Enter 10mL emulsifier tween 60 and 8mL Liquid Macrogol, stirring to formation solution B.
(3) solution B and activation hollow ceramic microspheres are mixed, moves into stainless steel hydrothermal reaction kettle, reacted at 230 DEG C
20h, cooled and filtered obtain solids B.
Step 3: heat treatment.
By solids B in 110 DEG C of dry 10h, then in 780 DEG C of calcining 3h, it is cooled to room temperature, it is net obtains lightweight bismuth tungstate
Change material.
The hollow ceramic microspheres are white ball, 26 μm of partial size, density 0.5g/cm3, compression strength 3.5 × 105Pa, than
Surface area 150m2/g。
The technical characteristics of the lightweight bismuth tungstate scavenging material of preparation are as follows: 30 μm of partial size, density 1.2g/cm3, resistance to compression
Intensity 3.3 × 105Pa, specific surface area 220m2/ g, refractoriness is less than 800 DEG C.
Claims (4)
1. a kind of preparation method of lightweight bismuth tungstate scavenging material, it is characterised in that the preparation method includes following processing steps:
Step 1: activation hollow ceramic microspheres；
1) NaOH solution of 50g hollow ceramic microspheres and the 0.3mol/L of 500mL are mixed, 65 DEG C is heated to, in this temperature
2h is kept the temperature, mixture A is obtained；
2) mixture A is filtered, is 7 with deionized water repeated flushing to filtrate pH value, obtains solids A；
3) it by solids A in 110 DEG C of dry 10h, then in 800 DEG C of calcining 3h, is cooled to room temperature, it is micro- to obtain activation hollow ceramic
Pearl；
Step 2: hydro-thermal overlay film；
1) 9 ~ 12g wolframic acid is dissolved in the NaOH solution of 0.5mol/L of 300mL, adds 10 ~ 15g, five nitric hydrate bismuth,
Stirring extremely forms solution A；
2) under stirring into solution A be added dropwise 0.5mol/L hydrochloric acid solution, adjust solution ph be 9, then be added 6 ~
10mL emulsifier and 5 ~ 8mL polyethylene glycol, stirring to formation solution B；
3) solution B and activation hollow ceramic microspheres are mixed, moves into stainless steel hydrothermal reaction kettle, in 210 ~ 230 DEG C of reaction 20h,
Cooled and filtered obtains solids B；
Step 3: heat treatment；
By solids B in 110 DEG C of dry 10h, then in 710 ~ 780 DEG C of calcining 3h, it is cooled to room temperature, it is net obtains lightweight bismuth tungstate
Change material.
2. a kind of preparation method of lightweight bismuth tungstate scavenging material according to claim 1, it is characterised in that the preparation side
Method includes following processing steps: the emulsifier is polysorbate60.
3. a kind of preparation method of lightweight bismuth tungstate scavenging material according to claim 1, it is characterised in that the preparation side
Method includes following processing steps: polyethylene glycol is Liquid Macrogol.
4. a kind of preparation method of lightweight bismuth tungstate scavenging material according to claim 1, it is characterised in that the preparation side
Method includes following processing steps: the hollow ceramic microspheres be ball, 8 ~ 26 μm of partial size, 0.5 ~ 0.6g/cm of density3, pressure resistance
Degree 3.5 × 105~4.0×105Pa, 150 ~ 180m of specific surface area2/g。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811143889.3A CN109248678B (en) | 2018-09-29 | 2018-09-29 | Preparation method of light bismuth tungstate purification material |
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| CN201811143889.3A CN109248678B (en) | 2018-09-29 | 2018-09-29 | Preparation method of light bismuth tungstate purification material |
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| CN109248678A true CN109248678A (en) | 2019-01-22 |
| CN109248678B CN109248678B (en) | 2021-05-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113788504A (en) * | 2021-09-30 | 2021-12-14 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113788504A (en) * | 2021-09-30 | 2021-12-14 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
| CN113788504B (en) * | 2021-09-30 | 2022-10-04 | 中国矿业大学 | Bismuth tungstate-based photocatalytic reactor and mineral processing wastewater degradation system |
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