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 PDF

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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
solution
preparation
hollow ceramic
bismuth tungstate
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CN109248678B (en
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张文杰
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Shenyang Ligong University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts 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
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/31Chromium, molybdenum or tungsten combined with bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
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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

A kind of preparation method of lightweight bismuth tungstate scavenging material
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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Cited By (1)

* Cited by examiner, † Cited by third party
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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CN101767002A (en) * 2009-01-01 2010-07-07 中国石油大学(北京) Method for synthesizing novel visible light driven BI2WO6 photocatalyst by employing microemulsion-hydrothermal technology
CN106669650A (en) * 2016-12-16 2017-05-17 池州方达科技有限公司 Pretreatment method of ceramic microspheres serving as catalyst carrier
CN107159183A (en) * 2017-06-05 2017-09-15 沈阳理工大学 A kind of preparation method and applications of the ceramic hollow microballon of metatitanic acid neodymium cladding
CN108355669A (en) * 2018-01-25 2018-08-03 太原理工大学 A kind of magnetic Nano onion carbon load Bi2WO6Photochemical catalyst and its preparation method and application

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Cited By (2)

* Cited by examiner, † Cited by third party
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
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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