CN115920826A - Red mud-based adsorbent and preparation method and application thereof - Google Patents
Red mud-based adsorbent and preparation method and application thereof Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000010802 sludge Substances 0.000 claims abstract description 38
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 25
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 23
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 41
- 229910052698 phosphorus Inorganic materials 0.000 claims description 41
- 239000011574 phosphorus Substances 0.000 claims description 41
- 239000000463 material Substances 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 9
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 229910019142 PO4 Inorganic materials 0.000 abstract description 12
- 239000010452 phosphate Substances 0.000 abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 10
- 239000002351 wastewater Substances 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 7
- 238000011084 recovery Methods 0.000 abstract 1
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- 239000000203 mixture Substances 0.000 description 9
- 239000002910 solid waste Substances 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 239000004568 cement Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
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- 230000000694 effects Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000012851 eutrophication Methods 0.000 description 4
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- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a red mud-based adsorbent, and a preparation method and application thereof. The method comprises the steps of carrying out roasting reaction I on red mud to obtain roasted red mud; mixing the roasted red mud with sludge of a water purification plant, water glass and water, and granulating to obtain raw material granules; and (3) sequentially carrying out steam curing treatment and roasting reaction II on the raw material particles to obtain the finished product. The adsorbent has high porosity and strong adsorption capacity, has higher purification efficiency when being applied to the dephosphorization of wastewater, can be recycled, has simple preparation method and low cost, and has important significance for solving the resource comprehensive utilization and the phosphate recovery of the red mud and the sludge of a water purification plant and realizing the 'treatment of wastes with processes of wastes against one another'.
Description
Technical Field
The invention relates to an adsorbent, in particular to a red mud-based adsorbent, and also relates to a preparation method and application thereof, belonging to the technical field of comprehensive utilization of solid wastes and wastewater purification.
Background
Nitrogen and phosphorus are key factors for limiting eutrophication of freshwater lakes, and excessive nutrient substances such as nitrogen and phosphorus in water can cause rapid propagation of algae and other plankton, decrease of water body dissolution, deterioration of water quality, and death of fishes and biomass thereof in large quantities. Phosphorus is a main element of eutrophication, the source of the phosphorus is divided into an external source part and an internal source part, and domestic sewage of residents and industrial and agricultural production sewage are main sources of the external phosphorus; while endogenous contamination is from phosphate released by the sediment. Therefore, in order to prevent the occurrence of water eutrophication, besides controlling the discharge of phosphorus at the source, it is important to find an economic and environment-friendly phosphorus removal adsorbent, wherein the method using minerals as the adsorbent is relatively cheap.
The red mud is waste residue discharged after alumina is refined in alumina industry, china is a large alumina production country, and the red mud produced each year is about more than 3000 million tons and accounts for more than 1/3 of the world. At present, most of alumina factories at home and abroad convey red mud to yards and store the red mud in dams, and the red mud not only occupies a large amount of land but also seriously deteriorates the ecological environment. Therefore, the resource utilization is imminent. The red mud contains a large amount of active metal oxides such as calcium, aluminum, iron, silicon and the like, and has a porous structure, so the red mud can be used for preparing adsorbent materials. Because the original red mud has weak phosphorus adsorption capacity, the phosphorus removal capacity of the red mud needs to be improved through modification.
The sludge of the water purification plant is an inevitable by-product in the process of producing tap water by the water purification plant, and the main components of the sludge are partly organic matters and inorganic matters in raw water and partly flocculating agents (aluminum salt and ferric salt are more) added into the water purification plant. The sludge of the water treatment plant is taken as garbage for long term and is not recycled. Because the water treatment plant sludge contains a large amount of amorphous iron and aluminum hydroxide, the characteristic makes the water treatment plant sludge have good adsorption effect on phosphorus.
However, at present, the solid wastes are not well utilized, and particularly, the solid wastes are not effectively utilized in the aspect of water body treatment, so that research on ways for fully recycling the solid wastes to prevent and control eutrophication of water bodies is urgently needed.
Disclosure of Invention
Aiming at the defects of low comprehensive utilization efficiency, incapability of combining water body phosphorus enrichment and the like of the existing sludge treatment technology of red mud and water purification plants, the invention aims to provide a red mud-based adsorbent which has high porosity and excellent adsorption performance, can efficiently adsorb phosphate, can release phosphorus through adding acid to a material adsorbing phosphorus, can be applied as a soil phosphate fertilizer, and can realize regeneration and utilization.
The second purpose of the invention is to provide a preparation method of the red mud-based adsorbent. The method takes the red mud and the sludge of the water purification plant as raw materials, effectively realizes the resource utilization of the solid waste, is simple, low in cost, green and environment-friendly, and is suitable for industrial production.
The third purpose of the invention is to provide the application of the red mud-based adsorbent. When the adsorbent is applied to the dephosphorization of wastewater, the purification efficiency is higher, the adsorbent can be regenerated and recycled, the purpose of treating wastes with processes of wastes against one another can be realized through the adsorbent, and the economic, social and environmental benefits are higher.
In order to realize the technical purpose, the invention provides a preparation method of a red mud-based adsorbent, which comprises the steps of carrying out roasting reaction I on red mud to obtain roasted red mud; mixing the roasted red mud with sludge of a water purification plant, water glass and water, and granulating to obtain raw material granules; and (3) sequentially carrying out steam curing treatment and roasting reaction II on the raw material particles to obtain the finished product.
The invention takes the red mud of the sintering method as the raw material, and can improve the removal efficiency of the red mud to phosphorus through roasting and activation. CaO and Al contained in red mud 2 O 3 And Fe 2 O 3 Can form insoluble precipitate with phosphate radical, al 2 O 3 Hydroxylation can also occur under a certain pH environment, and the effect of adsorption and condensation on phosphorus in water is generated. By roasting activation, the metal oxides such as CaO and SiO contained in the red mud 2 The components can form silicate with relatively stable structure, so that the strength of the formed red mud particles is obviously increased, and the capability of resisting hydraulic shock load is improved. In addition, in the roasting process of the red mud, existing hydrated minerals, carbonate minerals and the like are easily decomposed to release moisture or gas, and a porous structure is formed in the red mud, so that the specific surface area is increased. Functional groups formed by roasting and activating and oxides of calcium, iron and aluminum and the like inherently existing in the red mud can react with phosphate radicals, and the phosphorus removal process is characterized by surface functional group adsorption and surface chemical precipitation. The red mud prepared by the sintering method has low content of iron and aluminum oxides, is difficult to prepare a granular adsorbent, and has difficult phosphorus removal effect to meet the requirement, so the sludge of a water treatment plant is added, and the sludge of the water treatment plant is rich in a large amount of iron and aluminum oxides, so that the phosphorus removal efficiency can be further improved; and water glass is used as an excitant, and the steam curing of the mixture can promote the hydration reaction of the red mud base excited cementitious material, improve the quantity of C-S-H gel of reaction products, facilitate the forming and improve the material strength. The roasting treatment is carried out on the material after steam curing, the problem that the sludge of the water treatment plant in the material releases ammonia nitrogen and organic matters can be solved, and the phosphorus adsorption capacity of the sludge of the water treatment plant can be improved.
As a preferred scheme, the red mud is sintering process red mud.
As a preferable scheme, the conditions of the roasting reaction I are as follows: the temperature is 600-850 ℃, and the time is 1-3 h.
As a preferable scheme, the mass part ratio of the roasted red mud, the sludge of the water treatment plant and the water glass is 70-90: 10 to 30:5 to 15. In a further preferred scheme, the mass parts of the roasted red mud, the sludge of the water treatment plant and the water glass are 80-85: 10 to 20:5 to 10.
The mixing amount of the red mud, the sludge of the water treatment plant and the water glass is an important factor influencing the performance of the adsorption material. When the red mud mixing amount is too high, the formed gelled product is insufficient, the material strength is not enough, the material is not easy to form, and when the red mud mixing amount is too low, the phosphorus removal efficiency is low; when the sludge mixing amount of the water treatment plant is too high, the porosity of the material is reduced, the removal efficiency of phosphorus is influenced, and when the sludge mixing amount of the water treatment plant is too low, the strength of the material is insufficient, and the removal rate is relatively reduced; when the content of the water glass is too low, the material is easy to break, and when the content of the water glass is too high, the viscosity is increased, the operability is poor, and the phosphorus removal efficiency is relatively reduced.
Preferably, the modulus of the water glass is 2 to 3.0. The strength of the particle material can be improved by adding the water glass, and the water impact load resistance can be improved. The adsorbent with the optimal performance can be obtained by controlling the modulus of the water glass within a reasonable range. The modulus of the water glass can influence the cementing property of the adhesive, and has certain influence on the gelation time and the gel strength of the material. Generally, the higher the modulus, the stronger the adhesion, and the easier the hardening and film forming, but the water glass viscosity increases to some extent, and the workability becomes poor. Therefore, considering all together, the selection of water glass with modulus of 2.4-2.8 can make the material have the best overall performance.
As a preferable scheme, the mass of the water is 0.4 to 0.6 time of the total mass of the roasted red mud, the sludge of the water purification plant and the water glass. Controlling the amount of water in the appropriate range facilitates granulation to obtain a better adsorbent. When the water consumption is too high, the material is difficult to pelletize, the prepared raw material particles are easy to deform, and when the water consumption is too low, the roasted red mud, the water purification plant sludge and the water glass are difficult to bond and relatively difficult to form when mixed and pelletized.
As a preferable mode, the size of the raw material particles is 10 to 15mm.
As a preferred scheme, the steam curing treatment conditions are as follows: the temperature is 50-70 ℃ and the time is 24-60 h. The steam curing can promote the hydration reaction of the red mud base-activated cementing material and improve the quantity of C-S-H gel of reaction products, thereby leading the structure to be more compact and greatly improving the strength. When the temperature is too low and the time is too short, the gelled product is too small in quantity, insufficient in strength and not easy to form; the temperature is increased to promote the formation of a gelled product, and the strength of the gelled product is close to consistency after reaching a certain temperature and time.
As a preferred scheme, the conditions of the roasting reaction II are as follows: the temperature is 300-500 ℃ and the time is 2-4 h. Calcining the steam cured material to decomposeThe problem that the sludge in the water treatment plant releases ammonia nitrogen and organic matters in the material is solved, and the phosphorus adsorption capacity of the sludge in the water treatment plant can be improved. When the roasting temperature is too high and the roasting time is too long, the phosphorus adsorption capacity is reduced, mainly because the temperature is too high, and the internal Al (OH) is caused 3 Dehydroxylation, crystallization of amorphous substances in the material, and reduction of adsorption sites and phosphorus adsorption capacity after roasting under the two actions; when the roasting temperature is too low and the time is too short, the roasting effect cannot be achieved.
The invention also provides a red mud-based adsorbent, which is prepared by the method. The adsorbent has high porosity and excellent adsorption performance, can efficiently adsorb phosphate, and the material adsorbing phosphorus can release phosphorus through adding acid, and can be used as soil phosphate fertilizer for application, and the adsorbing material can realize recycling.
The invention also provides application of the red mud-based adsorbent, which is used as an adsorption material for adsorbing phosphorus substances in a water body. When the adsorbent is used as an adsorbing material for removing phosphorus from wastewater, the purification efficiency is higher, the purpose of treating waste by waste is achieved, and the economic, social and environmental benefits are higher.
Compared with the prior art, the invention has the following beneficial technical effects:
(1) The adsorbent has high porosity and excellent adsorption performance, particularly has higher adsorption efficiency on phosphate, can effectively solve the problem of phosphorus enrichment in water, and the material after phosphorus adsorption can release phosphorus, thereby being applied as a soil phosphate fertilizer and realizing the regeneration and utilization of the material.
(2) The preparation method is simple, mild in condition and low in cost, red mud and water treatment plant sludge are used as raw materials, so that the high-efficiency utilization of solid waste is realized, the problems of long-term accumulation of red mud and high water content and difficult dehydration of the water treatment plant sludge are solved, the pollution of the red mud and the water treatment plant sludge to the environment is avoided, and a new way is provided for the disposal and the cyclic utilization of solid waste.
(3) Greatly improves the comprehensive utilization efficiency of the red mud and the sludge solid waste of the water treatment plant, and has higher economic, social and environmental benefits.
Detailed Description
In order to facilitate understanding of the present invention, the technical solutions of the present invention will be further described with reference to the following embodiments, but the present invention is not limited thereto.
The chemical compositions of red mud and water treatment plant sludge are shown in tables 1 and 2
TABLE 1 chemical composition of Red mud
| Chemical composition | Al 2 O 3 | SiO 2 | Fe 2 O 3 | CaO | MgO | Na 2 O | TiO 2 | K 2 O | Others are |
| Sintering process red mud (%) | 5.49 | 18.35 | 13.50 | 40.93 | 0.76 | 2.30 | 3.03 | 0.23 | 15.71 |
TABLE 2 chemical composition of Water treatment plant sludge
| Chemical composition | Al 2 O 3 | SiO 2 | Fe 2 O 3 | MnO | CaO | Na 2 O | K 2 O | Loss on ignition |
| Water treatment plant sludge (%) | 23.01 | 24.14 | 5.10 | 1.05 | 11.86 | 6.08 | 2.87 | 23.75 |
Example 1
Placing a certain amount of red mud in a muffle furnace, roasting for 2 hours at 800 ℃, naturally cooling and taking out; according to the mass ratio of the red mud to the sludge of the water purification plant to the water glass of 85 percent: 10%:5 percent, adding a proper amount of deionized water, uniformly mixing according to the water-cement ratio of 0.5, and preparing raw material particles with the diameter of 10-15 mm by a granulator; steam curing the raw material particles at 60 ℃ for 48h; and roasting the particles subjected to steam curing for 3 hours at the temperature of 400 ℃ in a muffle furnace to prepare the red mud-based dephosphorizing adsorbent, which is applied to removing phosphate in wastewater.
1g of the phosphorus-removing adsorbent was weighed and put into 50mL of 50mg/L phosphorus-containing solution, and an adsorption test was performed in a constant temperature shaking box. Under the conditions that the temperature is 25 ℃, the operation time is 4h, and the vibration speed is 100r/min, the dephosphorization efficiency is 92.7 percent.
Example 2
Placing a certain amount of red mud in a muffle furnace, roasting for 2 hours at 800 ℃, naturally cooling and taking out; according to the mass ratio of the red mud to the sludge of the water purification plant to the water glass of 80%:15%:5 percent, adding a proper amount of deionized water, uniformly mixing according to the water-cement ratio of 0.5, and preparing raw material particles with the diameter of 10-15 mm by a granulator; steam curing the raw material particles at 60 ℃ for 48h; and roasting the particles subjected to steam curing for 3 hours at the temperature of 400 ℃ in a muffle furnace to prepare the red mud-based dephosphorizing adsorbent, which is applied to removing phosphate in wastewater.
1g of the phosphorus-removing adsorbent was weighed and put into 50mL of 50mg/L phosphorus-containing solution, and an adsorption test was performed in a constant temperature shaking box. Under the conditions that the temperature is 25 ℃, the operation time is 4 hours, and the vibration speed is 100r/min, the dephosphorization efficiency is 94.2 percent.
Example 3
Placing a certain amount of red mud in a muffle furnace, roasting for 2 hours at 800 ℃, naturally cooling and taking out; according to the mass ratio of the red mud to the sludge of the water purification plant to the water glass of 60%:35 percent: 5 percent, adding a proper amount of deionized water, uniformly mixing according to the water-cement ratio of 0.5, and preparing raw material particles with the diameter of 10-15 mm by a granulator; steam curing the raw material particles at 60 ℃ for 48h; and roasting the particles subjected to steam curing for 3 hours at the temperature of 400 ℃ in a muffle furnace to prepare the red mud-based dephosphorizing adsorbent, which is applied to removing phosphate in wastewater.
1g of the phosphorus removal adsorbent is weighed and put into 50mL of 50mg/L phosphorus-containing solution, and an adsorption test is carried out in a constant-temperature shaking box. Under the conditions that the temperature is 25 ℃, the operation time is 4h, and the vibration speed is 100r/min, the dephosphorization efficiency is 65 percent.
Comparative example 1
Placing a certain amount of red mud in a muffle furnace, roasting for 2 hours at 800 ℃, naturally cooling and taking out; according to the mass ratio of the red mud to the sludge of the water purification plant to the water glass of 85 percent: 15%:0 percent of the raw material is added with a proper amount of deionized water, the mixture is uniformly mixed according to the water-cement ratio of 0.5, and the mixture is made into raw material particles with the diameter of 10 to 15mm by a granulator; steam curing the raw material particles at 60 ℃ for 48h; and roasting the particles subjected to steam curing for 3 hours at the temperature of 400 ℃ in a muffle furnace to prepare the red mud-based dephosphorizing adsorbent, which is applied to removing phosphate in wastewater.
1g of the phosphorus removal adsorbent is weighed and put into 50mL of 50mg/L phosphorus-containing solution, and an adsorption test is carried out in a constant-temperature shaking box. Under the conditions that the temperature is 25 ℃, the operation time is 4h, and the vibration speed is 100r/min, the dephosphorization efficiency is 93.5 percent. The material is not strong enough, and the material is easy to be broken after being vibrated and can not be regenerated.
Comparative example 2
Placing a certain amount of red mud in a muffle furnace, roasting for 2 hours at 800 ℃, naturally cooling and taking out; according to the mass ratio of the red mud to the sludge of the water purification plant to the water glass of 95%:5%:0 percent of deionized water is added, the mixture is uniformly mixed according to the water-cement ratio of 0.5, and raw material particles with the diameter of 10-15 mm are prepared by a granulator; steam curing the raw material particles at 60 ℃ for 48h; and then placing the particles subjected to steam curing into a muffle furnace to be roasted for 3 hours at the temperature of 400 ℃, wherein the roasted material cannot be roasted and molded.
Example 4
The material after phosphorus removal in example 2 was desorbed and dried with 0.1mol/L hydrochloric acid solution, and then used in adsorption experiments, and after three continuous operations, the phosphorus removal rate was 60%. The material can be regenerated and used, and the dissolved phosphate can be reused as phosphate fertilizer.
Claims (10)
1. A preparation method of a red mud-based adsorbent is characterized by comprising the following steps: carrying out roasting reaction I on the red mud to obtain roasted red mud; mixing the roasted red mud with sludge of a water purification plant, water glass and water, and granulating to obtain raw material granules; and sequentially carrying out steam curing treatment and roasting reaction II on the raw material particles to obtain the finished product.
2. The method for preparing a red mud-based adsorbent according to claim 1, characterized in that: the conditions of the roasting reaction I are as follows: the temperature is 600-850 ℃, and the time is 1-3 h.
3. The method for preparing a red mud-based adsorbent according to claim 1 or 2, characterized in that: the mass parts of the roasted red mud, the sludge of the water purification plant and the water glass are 70-90: 10 to 30:5 to 15.
4. The method for preparing a red mud-based adsorbent according to claim 1 or 2, characterized in that: the modulus of the water glass is 2-3.0.
5. The method for preparing a red mud-based adsorbent according to claim 1, characterized in that: the mass of the water is 0.4-0.6 times of the total mass of the roasted red mud, the sludge of the water purification plant and the water glass.
6. The method for preparing a red mud-based adsorbent according to claim 1 or 5, characterized in that: the size of the raw material particles is 10-15 mm.
7. The method for preparing a red mud-based adsorbent according to claim 1, characterized in that: the steam curing treatment conditions are as follows: the temperature is 50-70 ℃ and the time is 24-60 h.
8. The method for preparing a red mud-based adsorbent according to claim 1, characterized in that: the conditions of the roasting reaction II are as follows: the temperature is 300-500 ℃ and the time is 2-4 h.
9. The red mud-based adsorbent is characterized in that: prepared by the process of any one of claims 1 to 8.
10. The use of the red mud-based adsorbent according to claim 9, wherein: the adsorbing material is used for adsorbing phosphorus substances in water.
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