CN110559984A - preparation method of red mud-based decolorizing material - Google Patents
preparation method of red mud-based decolorizing material Download PDFInfo
- Publication number
- CN110559984A CN110559984A CN201910785072.4A CN201910785072A CN110559984A CN 110559984 A CN110559984 A CN 110559984A CN 201910785072 A CN201910785072 A CN 201910785072A CN 110559984 A CN110559984 A CN 110559984A
- Authority
- CN
- China
- Prior art keywords
- red mud
- filter residue
- drying
- post
- sieving
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000007873 sieving Methods 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 18
- 238000004131 Bayer process Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 230000006872 improvement Effects 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 12
- 238000001179 sorption measurement Methods 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000005067 remediation Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000004042 decolorization Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 238000009776 industrial production Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 238000003828 vacuum filtration Methods 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- UGACIEPFGXRWCH-UHFFFAOYSA-N [Si].[Ti] Chemical compound [Si].[Ti] UGACIEPFGXRWCH-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 238000006065 biodegradation reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Treatment Of Sludge (AREA)
Abstract
A preparation method of a red mud-based decolorizing material comprises the following steps: (1) pretreating, namely drying the red mud, and sequentially crushing, grinding and sieving the dried red mud to obtain pretreated red mud powder; (2) acid leaching; (3) post-treatment, namely washing the red mud filter residue with water and then drying; (4) surface modification, mixing cetyl trimethyl ammonium bromide, ferric trichloride and urea to prepare an improved solution, and placing the improved solution and the post-treated red mud filter residue in a reaction container for reaction for at least 30 min. The red mud is separated and subjected to surface modification while the specific surface area of the red mud is increased, so that the red mud has certain selective adsorption capacity and can play a better role in the fields of environmental remediation and sewage treatment; therefore, on one hand, the environmental problem caused by stacking the red mud and a large amount of land occupied by stacking the red mud are solved, and on the other hand, the problems of decoloring and COD removal of the chroma wastewater can be solved.
Description
Technical Field
The invention relates to the field of materials for treating colored wastewater and printing wastewater, in particular to a preparation method of a red mud-based decolorizing material.
background
the red mud is used as polluting alkaline waste residue generated in the process of producing alumina in the aluminum production industry, 1-2 tons of red mud can be generated when 1 ton of alumina is produced, and at present, most alumina production enterprises at home and abroad convey the red mud to a red mud yard and generally divide the red mud into two types of damming wet-process stockpiling and dry-process stockpiling. The red mud needs a large amount of NaOH in the production process, is a mixture and has complex components, and the long-term stacking method can not only cause the seepage of harmful substances in the red mud, but also cause the salinization of underground water, thereby causing serious pollution to the environment. The comprehensive utilization of the red mud is realized, the red mud is turned into wealth, the environment-friendly material is formed, the industrial production can be realized, the additional value of the red mud is improved, a certain profit margin is created for enterprises, and the method is the best way for reducing the harm of the red mud.
The chroma waste water is also a very serious pollution in our daily life, and because the chroma is high, the components are complex, the toxicity is high, the photolysis is resisted, the biodegradation is difficult and the decolorization is difficult, the water quality is very complicated, the waste water contains a large amount of halides, nitro-compounds, aniline, phenols and the like, and a large amount of inorganic salts, and the substances easily cause serious pollution to the water. The method for treating the chroma waste water generally adopts methods such as an adsorption method, a flocculation sedimentation method, a biodegradation method, an oxidation decomposition method, a membrane separation method and the like, and the methods have advantages and disadvantages when treating the printing and dyeing waste water, wherein the adsorption method is to remove pollutants by utilizing the adsorption and fixation action of porous adsorption materials on the pollutants in the waste water, and the method is simple, fast, short in treatment time and high in efficiency and is a more method used in daily life.
The specific surface area of the red mud is small, so that the harmful substances in the red mud can be leaked out when the red mud is directly used, the adsorption effect cannot be achieved, and the water body can cause secondary pollution. In order to solve the problem, the red mud is subjected to component separation, and a porous silicon-titanium-based substance is separated to increase the specific surface area of the material, so that the red mud becomes an efficient decolorizing material, cannot cause secondary pollution when used in wastewater, is convenient to use and easy to recover, can adapt to industrial production, and has low production cost and higher added value. The method can reduce the pollution of the red mud to the environment and can also make the red mud become an environment-friendly material for restoring the environmental pollution, which is a very effective way for the comprehensive utilization of the red mud.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides the preparation method of the red mud-based decolorizing material, which is used for separating the red mud while increasing the specific surface area of the red mud and carrying out surface modification on the red mud so that the red mud has certain selective adsorption capacity and plays a better role in the fields of environmental remediation and sewage treatment.
the solution is that the preparation method of the red mud-based decolorizing material comprises the following steps:
(1) pretreating, namely drying the red mud, and sequentially crushing, grinding and sieving the dried red mud to obtain pretreated red mud powder;
(2) Acid leaching, namely placing the pretreated red mud powder and hydrochloric acid in a closed container, stirring and reacting for at least 5min at the temperature of 2-105 ℃, and performing solid-liquid separation to obtain red mud filter residue;
(3) Post-treatment, namely washing the red mud filter residue with water and then drying, crushing and sieving the dried red mud filter residue to prepare post-treatment red mud filter residue;
(4) Surface modification, namely mixing cetyl trimethyl ammonium bromide, ferric trichloride and urea to prepare an improvement solution, placing the improvement solution and post-treated red mud filter residue in a reaction container for reaction for at least 30min, filtering and cleaning the prepared improvement red mud, and finally drying, grinding and sieving in sequence to obtain the red mud-based decolorizing material.
Preferably, in the step (1), the red mud is bayer process red mud; the drying temperature is 80-110 ℃, and the moisture content of the dried red mud is less than or equal to 5%.
Preferably, in the step (2), the concentration of hydrochloric acid is 2-12 mol/L, and the ratio of the mass of the pretreated red mud powder to the volume of the hydrochloric acid is 1: 2-1: 10.
Preferably, in the step (3), the pH value of the post-treated red mud filter residue is 6-7.
Preferably, in step (1), the sieved screen is an 80-mesh screen.
Preferably, in the step (3), the drying temperature is 80-110 ℃; the sieved screen is a 40-mesh screen.
preferably, in the step (4), the drying temperature is 80-110 ℃, and the sieved screen is a 40-mesh screen.
preferably, in the step (4), the reaction temperature of the improving solution and the post-treated red mud filter residue is 100-120 ℃.
preferably, in step (3), the deionized water used is washed with water.
compared with the prior art, the invention has the beneficial effects that:
In order to change the red mud into valuable, make the micro waste solid waste red mud into an environment-friendly material, realize the industrial production and feasible industrial use of the red mud, and utilize useful components, such as SiO, contained in the red mud2、TiO2The red mud is separated while the specific surface area of the red mud is increased, and is subjected to surface modification, so that the red mud has certain selective adsorption capacity and can play a better role in the fields of environmental remediation and sewage treatment; therefore, the problems of environmental problems caused by red mud stacking and large amount of land occupied by red mud stacking are solved, the problems of color removal and COD removal of the chroma wastewater can be solved, the comprehensive utilization and environment-friendly development of the red mud are realized, and a green door is opened for the development of alumina of aluminum production enterprises.
drawings
FIG. 1 is a scanning electron microscope image of the original Bayer process red mud of the invention.
FIG. 2 is a scanning electron microscope image of red mud filter residue obtained by leaching Bayer process red mud with hydrochloric acid.
FIG. 3 is a scanning electron microscope image of the red mud-based decolorizing material.
Detailed Description
the following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Example 1
A preparation method of a red mud-based decolorizing material comprises the following steps:
(1) Pretreating, namely drying the red mud, and sequentially crushing, grinding and sieving the dried red mud to obtain pretreated red mud powder;
(2) Acid leaching, namely placing the pretreated red mud powder and hydrochloric acid in a closed container, stirring and reacting for at least 5min at the temperature of 2-105 ℃, and performing solid-liquid separation to obtain red mud filter residue;
(3) Post-treatment, namely washing the red mud filter residue with water and then drying, crushing and sieving the dried red mud filter residue to prepare post-treatment red mud filter residue;
(4) surface modification, namely mixing cetyl trimethyl ammonium bromide, ferric trichloride and urea to prepare an improvement solution, placing the improvement solution and post-treated red mud filter residue in a reaction container for reaction for at least 30min, filtering and cleaning the prepared improvement red mud, and finally drying, grinding and sieving in sequence to obtain the red mud-based decolorizing material.
In the step (1), the red mud is Bayer process red mud; the drying temperature is 80-110 ℃, the moisture content of the dried red mud is less than or equal to 5%, and a sieving screen is a 80-mesh sieve.
In the step (2), the concentration of hydrochloric acid is 2-12 mol/L, and the ratio of the mass of the pretreated red mud powder to the volume of the hydrochloric acid is 1: 2-1: 10.
In the step (3), the drying temperature is 80-110 ℃; the sieved screen mesh is a 40-mesh screen mesh, and deionized water is adopted for washing.
In the step (4), the drying temperature is 80-110 ℃, the sieved screen is a 40-mesh screen, and the reaction temperature of the improved solution and the post-treatment red mud filter residue is 100-120 ℃.
Example 2
Placing a 500mL three-neck round-bottom flask in a constant-temperature electric heating cap, connecting a stirrer, cooling the solution in the three-neck round-bottom flask by a condenser pipe filled with cooling water, adding 40g Bayer process red mud and 200mL 12mol/L hydrochloric acid into the three-neck flask, setting the temperature of the constant-temperature heating cap at 65 ℃, setting the rotating speed of the stirrer at 500r/min, and setting the reaction time to be 1 h; after the reaction is finished, pouring the turbid liquid into a vacuum filtration bottle for solid-liquid separation, cleaning the separated red mud filter residue solid with deionized water to be nearly neutral, drying, crushing and grinding the solid, sieving with a 80-mesh sieve to obtain a red mud filter residue sample, and storing the red mud filter residue sample in a closed container;
Adding 1g of ferric trichloride, 1g of hexadecyl trimethyl ammonium bromide solid and 1g of urea solid particles into a 1L volumetric flask, adding distilled water to a constant volume of 1L, shaking up, and dissolving the solid to obtain a modified solution; adding 10g of treated red mud filter residue into 1L of modified liquid, putting the modified liquid into a pressure container, heating the pressure container to 107-111 ℃, preserving the heat for 1h, cooling the container, filtering the solution, drying the filter residue for 12h at 105 ℃, grinding the filter residue through a 80-mesh sieve to obtain modified red mud filter residue, and sealing and storing the modified red mud filter residue to prevent the filter residue from being affected with damp.
Example 3
Placing a 500mL three-neck round-bottom flask in a constant-temperature electric heating cap, connecting a stirrer, cooling the solution in the three-neck round-bottom flask by a condenser pipe filled with cooling water, and adding 40g of original Bayer process red mud and 200mL of 12mol/L hydrochloric acid into the three-neck flask; setting the temperature of a constant-temperature heating cap to be 65 ℃, the rotating speed of a stirrer to be 500r/min, and the reaction time to be 1 h; and after the reaction is finished, pouring the turbid liquid into a vacuum filtration bottle for solid-liquid separation, cleaning the separated red mud filter residue solid with deionized water to be nearly neutral, drying, crushing and grinding the solid, sieving with a 80-mesh sieve to obtain a red mud filter residue sample, and storing the red mud filter residue sample in a closed container.
Adding 1g of ferric trichloride, 1g of hexadecyl trimethyl ammonium bromide and 1g of urea solid particles into a 1L volumetric flask, adding distilled water to a constant volume of 1L, shaking up until the solid is dissolved to obtain a modified solution; weighing 10g of red mud acid leaching residue, adding into 1L of modified liquid, placing into a pressure container, heating to 107-111 ℃, preserving heat for 1h, cooling along with the container, filtering the solution, drying filter residue for 12h at 105 ℃, grinding and sieving with a 80-mesh sieve to obtain modified red mud filter residue, namely the red mud-based decolorizing material, and sealing and storing to prevent moisture.
Example 4
Placing a 500mL three-neck round-bottom flask in a constant-temperature electric heating cap, connecting a stirrer, introducing a cooling water condenser pipe, and adding 40g of original Bayer process red mud and 200mL of 12mol/L hydrochloric acid into the three-neck flask; setting the temperature of a constant-temperature heating cap to be 65 ℃, the rotating speed of a stirrer to be 500r/min, and the reaction time to be 1 h; after the reaction is finished, pouring the turbid liquid into a vacuum filtration bottle for solid-liquid separation, cleaning the solid with deionized water to be nearly neutral, drying, crushing and grinding the solid, sieving with a 80-mesh sieve to obtain a red mud filter residue sample, and storing the red mud filter residue sample into a closed container;
Adding 1g of ferric trichloride, 1g of hexadecyl trimethyl ammonium bromide and 1g of urea solid particles into a 1L volumetric flask, adding distilled water to a constant volume of 1L, shaking up, and dissolving the solid to obtain the modified liquid. Weighing 10g of red mud acid leaching residue, adding into 1L of modified liquid, placing into a pressure container, heating to 107-111 ℃, preserving heat for 1h, cooling along with the container, filtering the solution, drying filter residue for 12h at 105 ℃, grinding and sieving with a 80-mesh sieve to obtain modified red mud filter residue, namely the red mud-based decolorizing material, and sealing and storing to prevent moisture.
results and analysis
(1) Analysis by scanning Electron microscope
As can be seen from FIG. 1, the original Bayer process red mud has very loose external appearance, different surface structures and no obvious crystal structure, which indicates that the original Bayer process red mud has various components and no regular and recyclable appearance due to the mixture; as can be seen from FIG. 2, the components of the Bayer process red mud residue after hydrochloric acid leaching are mostly observed to be in a small flaky structure, which indicates that the components are mostly the mixture of silicon dioxide and titanium dioxide, and the impurity content is greatly reduced; as can be seen from fig. 3, the morphology of the modified red mud filter residue, i.e., the red mud-based decolorization material, is the same as that of bayer red mud acid leaching residue, which indicates that the crystal structures in the original red mud are not damaged in the modification process, but the crystal structures are crosslinked with each other and are connected more tightly.
(2) X-ray fluorescence spectroscopy
TABLE 1X-ray fluorescence spectrum analysis results of the original Bayer process red mud and Bayer process red mud acid leaching residue
As is clear from Table 1, large amounts of CaO and Fe2O3、Al2O3Is leached out, a large amount of SiO is left2And TiO2The composition change in the red mud is more clearly reflected, and the leaching rate of the red mud in the Bayer process is found to be 60-65% in experiments, so that the leaching rate is very high, which indicates that the content of the mixture in the red mud is very high.
(3) decolorization ratio
And (3) taking 20mL of acid red solution with the concentration of 50ppm, weighing 0.05g of modified red mud filter residue prepared in the example 2, adding the modified red mud filter residue into the solution, shaking the solution at room temperature for 3 hours, and then carrying out centrifugal filtration on the solution to obtain the decolorization rate of 99.64 percent.
And taking 20mL of wastewater with the concentration of 1063mg/g, weighing 0.02g of modified red mud filter residue prepared in example 3, adding the modified red mud filter residue into the solution, digesting the solution at 150 ℃ for 2 hours, and measuring the COD value of the wastewater to be 807mg/g after the solution is cooled to room temperature, wherein the removal amount of the COD reaches 25.4 mg/g.
And (3) taking 20mL of acid red solution with the concentration of 50ppm, weighing 0.05g of modified red mud filter residue prepared in example 4, adding the modified red mud filter residue into the solution, shaking the solution at room temperature for 0.5h, and then carrying out centrifugal filtration on the solution to obtain the decolorization rate of 99.06%.
The invention takes red mud as basic raw material, and takes silicon-titanium-based inorganic material as basic molecular skeleton to synthesize the high-efficiency decolorizing material through the reaction of acid leaching and surface modification of the red mud. The material contains high-silicon high-titanium porous groups and NH modified on the surface of the material4 +、CONH2 +The red mud-based decolorizing material has the advantages of simple production mode, low production cost, good decolorizing effect, high decolorizing efficiency and wide application in daily life and industrial production.
the above-mentioned embodiments do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention by those skilled in the art should be included in the protection scope defined by the claims of the present invention without departing from the design concept of the present invention.
Claims (5)
1. a preparation method of a red mud-based decolorizing material comprises the following steps:
(1) Pretreating, namely drying the red mud, and sequentially crushing, grinding and sieving the dried red mud to obtain pretreated red mud powder;
(2) Acid leaching, namely placing the pretreated red mud powder and hydrochloric acid in a closed container, stirring and reacting for at least 5min at the temperature of 2-105 ℃, and performing solid-liquid separation to obtain red mud filter residue;
(3) Post-treatment, namely washing the red mud filter residue with water and then drying, crushing and sieving the dried red mud filter residue to prepare post-treatment red mud filter residue;
(4) Surface modification, namely mixing cetyl trimethyl ammonium bromide, ferric trichloride and urea to prepare an improvement solution, placing the improvement solution and post-treated red mud filter residue in a reaction container for reaction for at least 30min, filtering and cleaning the prepared improvement red mud, and finally drying, grinding and sieving in sequence to obtain the red mud-based decolorizing material.
2. the method for preparing the red mud-based discoloring material as claimed in claim 1, wherein in the step (1), the red mud is bayer process red mud; the drying temperature is 80-110 ℃, the moisture content of the dried red mud is less than or equal to 5%, and a sieving screen is a 80-mesh sieve.
3. The method for preparing the red mud-based decolorizing material according to claim 1, characterized in that, in the step (2), the concentration of hydrochloric acid is 2-12 mol/L, and the ratio of the mass of the pretreated red mud powder to the volume of the hydrochloric acid is 1: 2-1: 10.
4. The preparation method of the red mud-based decolorizing material according to claim 1, characterized in that, in the step (3), the drying temperature is 80-110 ℃; the sieved screen mesh is a 40-mesh screen mesh, and deionized water is adopted for washing.
5. The preparation method of the red mud-based decolorizing material according to claim 1, characterized in that, in the step (4), the drying temperature is 80-110 ℃, the sieved screen is a 40-mesh screen, and the reaction temperature of the improving solution and the post-treatment red mud filter residue is 100-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910785072.4A CN110559984A (en) | 2019-08-23 | 2019-08-23 | preparation method of red mud-based decolorizing material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910785072.4A CN110559984A (en) | 2019-08-23 | 2019-08-23 | preparation method of red mud-based decolorizing material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110559984A true CN110559984A (en) | 2019-12-13 |
Family
ID=68776075
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910785072.4A Pending CN110559984A (en) | 2019-08-23 | 2019-08-23 | preparation method of red mud-based decolorizing material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110559984A (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1981921A (en) * | 2005-12-14 | 2007-06-20 | 中国科学院生态环境研究中心 | High-activity mud adsorbent and its production |
| US20080209968A1 (en) * | 2002-08-27 | 2008-09-04 | Nauveau Technology Investments Ltd. | Processes for Treatment of Wastewater, Separation, Deodorisation and Re-Use of Biosolids |
| US20100243568A1 (en) * | 2006-03-23 | 2010-09-30 | J.I. Enterprises, Inc. | Method of Sorbing Discolored Organic Compounds from Water |
| CN103706338A (en) * | 2014-02-10 | 2014-04-09 | 河南理工大学 | Red mud adsorbent for removing organic dye pollutants, and preparation method of adsorbent |
| CN106669751A (en) * | 2016-12-30 | 2017-05-17 | 东莞市联洲知识产权运营管理有限公司 | High-efficiency treatment method of methylene blue dye wastewater |
| CN107262019A (en) * | 2017-08-22 | 2017-10-20 | 同济大学 | A kind of changed red mud and its preparation method and application |
| CN108031443A (en) * | 2017-11-23 | 2018-05-15 | 浙江海洋大学 | A kind of preparation and its application of chromate waste water inorganic agent |
| CN109847704A (en) * | 2019-01-18 | 2019-06-07 | 昆明理工大学 | A kind of method and application preparing heavy metal chromium adsorbent using Dian Chi Dredged bed mud |
-
2019
- 2019-08-23 CN CN201910785072.4A patent/CN110559984A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080209968A1 (en) * | 2002-08-27 | 2008-09-04 | Nauveau Technology Investments Ltd. | Processes for Treatment of Wastewater, Separation, Deodorisation and Re-Use of Biosolids |
| CN1981921A (en) * | 2005-12-14 | 2007-06-20 | 中国科学院生态环境研究中心 | High-activity mud adsorbent and its production |
| US20100243568A1 (en) * | 2006-03-23 | 2010-09-30 | J.I. Enterprises, Inc. | Method of Sorbing Discolored Organic Compounds from Water |
| CN103706338A (en) * | 2014-02-10 | 2014-04-09 | 河南理工大学 | Red mud adsorbent for removing organic dye pollutants, and preparation method of adsorbent |
| CN106669751A (en) * | 2016-12-30 | 2017-05-17 | 东莞市联洲知识产权运营管理有限公司 | High-efficiency treatment method of methylene blue dye wastewater |
| CN107262019A (en) * | 2017-08-22 | 2017-10-20 | 同济大学 | A kind of changed red mud and its preparation method and application |
| CN108031443A (en) * | 2017-11-23 | 2018-05-15 | 浙江海洋大学 | A kind of preparation and its application of chromate waste water inorganic agent |
| CN109847704A (en) * | 2019-01-18 | 2019-06-07 | 昆明理工大学 | A kind of method and application preparing heavy metal chromium adsorbent using Dian Chi Dredged bed mud |
Non-Patent Citations (2)
| Title |
|---|
| MEHDI SHIRZAD-SIBONI ET AL.: "Removal of acid blue 113 and reactive black 5 dye from aqueous solutions by activated red mud", 《JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY》 * |
| 郑水林: "《粉体表面改性》", 30 June 2019, 中国建材工业出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104874365B (en) | Carboxymethyl cellulose ion insertion hydrotalcite-like composite material and preparation method and application | |
| CN109603856B (en) | Method for preparing Erdite rod-shaped particles from wastewater and applying Erdite rod-shaped particles to water treatment | |
| CN102936019A (en) | Method for preparing magnetic 4A molecular sieve by using kaolin | |
| CN111943336A (en) | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof | |
| CN102127639A (en) | Preparation method of high-clarity uranium solution | |
| CN101486769A (en) | Preparation of amidoxime group bacteria cellulose | |
| CN107089786B (en) | Method for improving municipal sludge dewatering effect by using aluminum ash | |
| CN107042088A (en) | Preparation method for the modified bentonite adsorbent of waste water decoloration of cation dyes | |
| CN105771920B (en) | A kind of preparation method of the alkali lignin adsorbing material of sodium glutamate modification and its application in removing waste water dyestuff | |
| CN110721655A (en) | Preparation method of heavy metal adsorbent based on red mud | |
| CN105001381B (en) | A kind of preparation method of paper mill sludge base Amphiphatic high polymer coagulant | |
| CN1850607A (en) | Method for preparing iron-free aluminium sulfate and superfine active carbon white utilizing aluminium first-class ore | |
| CN101579685A (en) | Method for processing and utilizing electrolytic manganese waste residue | |
| CN110559984A (en) | preparation method of red mud-based decolorizing material | |
| CN104857931A (en) | Production method of printing and dyeing wastewater adsorption, flocculation and photocatalysis materials | |
| CN104826577A (en) | Modified slag adsorbent for anion dye wastewater treatment, and preparation method thereof | |
| CN115571922A (en) | Process for recovering sodium carbonate and magnetic iron oxide from red mud by using carbon dioxide | |
| CN115477948A (en) | Method for preparing FeOOH modified coal gangue by utilizing red mud | |
| CN114873901A (en) | Preparation method of novel sludge conditioner applied to plate-and-frame filter press | |
| CN109179615B (en) | Modified cotton fiber adsorbent for removing nitrate nitrogen and preparation method and application thereof | |
| CN107398256A (en) | A kind of magnetic stalk quaternary ammonium salt/rectorite compound material and preparation method thereof | |
| CN106192532A (en) | A kind of sludge modification and reuse method | |
| CN102092753B (en) | Alcoholization removing method of impurity iron in aluminum sulfate solution | |
| CN106517265A (en) | Recycling utilization method of biochemical sludge | |
| CN111762791A (en) | Method for preparing flocculating agent by utilizing furnace slag and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191213 |