CN114011375B - Preparation of granular phosphorus removing agent by titanium gypsum resource utilization - Google Patents
Preparation of granular phosphorus removing agent by titanium gypsum resource utilization Download PDFInfo
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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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- 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
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The invention relates to a resource utilization technology of industrial byproduct gypsum solid waste, in particular to a technology for preparing a granular phosphorus removing agent by resource utilization of titanium gypsum. The method comprises the following steps of taking titanium gypsum waste residue generated in the production process of titanium dioxide as a main raw material, taking dewatered sludge generated in the sewage treatment process as an auxiliary raw material, mixing the main raw material and a proper amount of auxiliary raw material and placing the main raw material and the proper amount of auxiliary raw material in the same porcelain boat, or placing the main raw material and the proper amount of auxiliary raw material in different porcelain boats respectively, roasting at high temperature under nitrogen atmosphere, drying and grinding to prepare powdery phosphorus removal agents I and II respectively; and then mixing the powdery phosphorus removal agent I or II with a small amount of adhesive and water, kneading into clusters, extruding, cutting into columnar particles, and drying to obtain the granular phosphorus removal agent. The granular phosphorus removal agent is prepared from the titanium gypsum and the sludge, so that the problem of treatment of industrial byproduct gypsum waste residues and sludge of sewage treatment plants can be effectively solved, and the prepared granular phosphorus removal agent can be used for purification treatment of various phosphorus-polluted water bodies, and waste is changed into valuable. The method disclosed by the invention has wide application prospects in the fields of titanium gypsum resource utilization and phosphorus-polluted water purification.
Description
Technical Field
The invention relates to a granular phosphorus removing agent prepared by titanium gypsum resource utilization, belonging to the field of titanium gypsum resource utilization and the field of phosphorus-polluted water purification.
Background
Titanium gypsum (yellow gypsum, red gypsum, commonly called yellow mud) is an industrial byproduct gypsum obtained by adding lime (or carbide slag) for neutralization in a process of producing titanium dioxide by a sulfuric acid method in titanium dioxide production enterprises, and the main components of the gypsum are calcium sulfate dihydrate, ferrous/iron sulfate, oxide, titanium oxide and the like. Because of the factors of high water content, high viscosity, complex components, fine particles and the like, the titanium gypsum is one of the most difficult resource utilization in the industrial byproduct gypsum solid waste at present. According to relevant data statistics, the titanium gypsum has an output of nearly 3000 ten thousand tons every year in China, but the comprehensive utilization rate is only 10%, and more than 1.3 million tons of titanium gypsum are only stacked in the open air, so that on one hand, a large amount of land and resources are wasted, and on the other hand, the environmental and geological safety problems caused by long-term accumulation of the titanium gypsum are increasingly obvious. The resource utilization of titanium gypsum becomes a great problem affecting the sustainable development of titanium dioxide enterprises. At present, the research on the titanium gypsum resource utilization technology at home and abroad mainly focuses on the utilization of titanium gypsum as a cement retarder, a composite cementing material, a soil conditioner, a carbon dioxide collector, the production of high-quality calcium sulfate and the like. However, due to the small amount of use, high production cost, low added value of products and the like, there are reports of large-scale application, and a resource utilization method which is efficient, environment-friendly and large in treatment capacity needs to be found and established urgently.
Phosphorus is one of the main factors of water eutrophication, and the removal of phosphate from the eutrophic water is a global environmental problem. In recent years, some calcium-rich natural minerals (e.g., dolomite, calcite) and industrial by-product materials (e.g., waste concrete, oil shale) have been used as sorbent materials for phosphate removal. Gypsum is also used as a calcium-rich mineral as a phosphorus-removing adsorbent, but the adsorption capacity of unactivated gypsum to phosphorus is very limited, and for example, studies by Yao Jingjun et al (water treatment technology, 2009,35,44) and Cong Haibing et al (environmental technology, 2014,27,20-27) have found that the saturated adsorption capacity of homemade gypsum and commercially available gypsum (medical gypsum and gypsum for construction) to phosphorus in water is less than 1mg/g. The phosphorus adsorption capacity of gypsum can be effectively improved by activating and modifying the gypsum or compounding the gypsum with other materials, for example, cheng Peng (the university of fertility industry, 2018), magnesite calcined in 800 ℃ air atmosphere is compounded in anhydrite ore, or desulfurized gypsum is subjected to heat treatment in air atmosphere (400-800 ℃), and the saturated adsorption capacity of the prepared series of phosphorus removal materials to phosphorus can be improved to be nearly 30mg/g; qiu Xuejian (2015 university of Guizhou, master academic paper) prepares the phosphogypsum whisker with the saturated adsorption quantity of phosphorus up to 140mg/g by carrying out hydrothermal treatment on phosphogypsum waste residue; the patent 'a method for removing acid phosphorus-containing wastewater by using modified fluorgypsum' (201510952328.8) prepares a dephosphorizing wastewater adsorbent which can be used for purifying acid phosphorus-containing wastewater of phosphorus chemical enterprises by carrying out multi-step treatment on fluorgypsum waste residues through soaking of spinach oxalic acid leach liquor, barium hydroxide reaction, high-temperature calcination under air atmosphere, soaking of sodium hydroxide, sea salt precipitation, secondary high-temperature calcination and the like; the patent 'biomass carbon-based desulfurized gypsum phosphorus removal rod and the preparation and use methods thereof' (201811050641.2) is characterized in that desulfurized gypsum, crop straws or sawdust, vegetable oil and other raw materials are mixed and extruded into a rod, and the rod is carbonized at high temperature in vacuum atmosphere to prepare the biomass carbon-based desulfurized gypsum phosphorus removal rod which can be used for reducing, removing and fixing phosphorus in various phosphorus-rich polluted water bodies and soil.
The invention provides a simple and feasible method for preparing a granular phosphorous removing agent by resource utilization of titanium gypsum. Titanium gypsum waste residue generated in the production process of titanium dioxide is used as a main raw material, a proper amount of sludge of a sewage treatment plant is mixed and roasted in the titanium gypsum, or the activation effect of gas generated in the roasting process of the sludge on the titanium gypsum is utilized to prepare a series of powdery phosphorus removing agents, and then the granular phosphorus removing agents are prepared by extrusion, cutting and drying. The granular phosphorus removing agent has excellent adsorption performance on phosphorus in a water body, and the application form is flexible. The granular phosphorus removal agent is prepared from the titanium gypsum and the sludge, so that the problem of treatment of industrial byproduct gypsum waste residues and sludge of sewage treatment plants can be effectively solved, and the prepared granular phosphorus removal agent can be used for purification treatment of various phosphorus-polluted water bodies.
Disclosure of Invention
The invention aims to provide a method for preparing a granular phosphorus removing agent by resource utilization of titanium gypsum aiming at the problems of treatment of titanium gypsum solid waste and purification of phosphorus-polluted water.
In order to realize the purpose of the invention, the technical scheme is as follows: (1) Drying and grinding titanium gypsum waste residues generated in the production process of titanium dioxide to obtain a main raw material G; (2) Drying and grinding dewatered sludge generated in the sewage treatment process to obtain an auxiliary raw material S; (3) Mixing a main raw material G and a proper amount of an auxiliary raw material S, placing the mixture in the same porcelain boat, roasting at a high temperature in a nitrogen atmosphere, drying and grinding to prepare a powdery phosphorus removal agent I; or respectively placing the main raw material G and a proper amount of the auxiliary raw material S in different porcelain boats, roasting at high temperature under nitrogen atmosphere, drying, mixing and grinding to prepare a powdery phosphorus removal agent II; (4) Mixing the powdery phosphorus removal agent I or II with a small amount of adhesive and water, kneading into a cluster, then extruding and cutting into columnar particles, and drying to obtain the granular phosphorus removal agent.
The main raw material titanium gypsum is derived from the dilute acid neutralization process of titanium dioxide production enterprises, and the main components are calcium sulfate dihydrate (60-80 wt%), iron oxide (10-20 wt%), titanium oxide (1-5 wt%) and other impurities; the auxiliary raw material dewatered sludge is sourced from municipal sewage treatment plants, papermaking sewage treatment plants or industrial park sewage treatment plants, and the content of organic matters in the solid is 35-55wt%; the adding proportion of the auxiliary raw materials is 2-50wt% of the sum of the weight of the main raw materials and the auxiliary raw materials; the high-temperature roasting temperature is 600-800 ℃.
The used adhesive is one or more of methylcellulose, carboxymethylcellulose and bentonite, and the adding proportion of the adhesive is 1-10% of the weight of the powdery phosphorus removing agent; the diameter of the prepared columnar granular dephosphorizing agent is 1-2mm, and the length is 4-6mm.
The application method of the granular phosphorus removing agent prepared by the invention comprises the following steps: directly adding the granular phosphorus removing agent into a phosphorus-polluted water body, and carrying out solid-liquid separation after reacting for a certain time; or the granular phosphorus removing agent is filled into an adsorption column, and the phosphorus-polluted water body passes through an adsorption bed layer at a certain flow rate to be purified; or the granular phosphorus removing agent is used as ecological bank protection filler for purifying surface runoff into a river/reservoir/lake, the phosphorus-containing surface runoff is purified when flowing through the filler, and the filler rich in phosphorus can be used as phosphate fertilizer to promote plant growth.
The innovation points of the invention are as follows: by directly adding sludge roasting into the titanium gypsum solid waste or indirectly utilizing the activation effect of gas generated in the sludge roasting process on the titanium gypsum and combining the conventional extrusion granulation process, the titanium gypsum which is difficult to be comprehensively utilized is converted into a granular dephosphorizing agent with high-efficiency adsorption performance on phosphorus in the water body, so that the resource utilization problem of the titanium gypsum is solved on one hand, and the purification of the phosphorus-polluted water body is realized on the other hand.
The invention has the beneficial effects that: (1) The titanium gypsum generated in the production process of titanium dioxide is used as a main raw material, the sludge generated in the sewage treatment process is used as an auxiliary raw material, and the efficient and stable granular phosphorus removing agent is prepared by simple treatments such as drying, high-temperature roasting, extrusion granulation and the like, so that the treatment and disposal problems of the titanium gypsum and the sludge can be effectively solved, and the purpose of changing waste into valuable is achieved; (2) The granular phosphorus removing agent prepared by the invention has the saturated adsorption capacity of phosphorus up to 160mg/g, has excellent mechanical property, can be applied in various modes such as directly adding phosphorus-polluted water, filling into an adsorption column, setting into a permeable reaction wall for purifying surface runoff of rivers and lakes and the like, and can effectively solve the purification problem of the phosphorus-polluted water; (3) The granular phosphorus removal agent prepared by the titanium gypsum resource utilization disclosed by the invention has the advantages of wide raw material source, low treatment cost, environmental friendliness and the like, utilizes solid wastes such as titanium gypsum, sludge and the like which are difficult to treat, can be used for purifying phosphorus-polluted water bodies, and has wide application prospects in the field of titanium gypsum resource utilization and the field of phosphorus-polluted water body purification.
Drawings
FIG. 1 is an optical photograph of a phosphorus removing agent in the form of columnar particles prepared according to the present invention;
FIG. 2 is an electron microscope (SEM) photograph of the granular phosphorus removal agent after purifying a phosphorus-contaminated water body;
FIG. 3 is an EDS elemental analysis of the particle phosphorous removal agent after purifying a phosphorous-contaminated water body.
Detailed Description
To better illustrate the invention, the following examples are given:
example 1:
placing the dried titanium gypsum in a porcelain boat, roasting the titanium gypsum in a tube furnace in nitrogen atmosphere at 800 ℃ for 2 hours, and naturally cooling the titanium gypsum to room temperature to obtain powdery phosphorus removing agent GS 0 -800。
30mg of GS 0 800 to 30mL of polluted water containing 5 to 200mg/L of phosphorus for carrying out phosphorus static adsorption experiment. The results of the study showed that GS 0 -800 has a saturated adsorption capacity for phosphorus of less than 5mg/g.
Example 2:
placing the dried titanium gypsum and equivalent municipal sludge into two different porcelain boats respectively, roasting the titanium gypsum and equivalent municipal sludge in the same tubular furnace in nitrogen atmosphere at 800 ℃ for 2 hours, naturally cooling the titanium gypsum and the municipal sludge to room temperature, and placing the titanium gypsum and the porcelain boats to obtain a product, namely the powdery phosphorus removal agent GS m0 -s-800. Mixing GS m0 Mixing-s-800 with 1wt% of methylcellulose and 30wt% of water, kneading into clusters, performing extrusion molding, cutting into columnar particles, and drying to obtain the granular phosphorus removal agent PGS m0 -s-800。
30mg of PGS m0 And (4) s-800, adding the mixture into 30mL of polluted water containing 5-200mg/L of phosphorus, and performing a phosphorus static adsorption experiment. The results of the study showed that PGS m0 The saturated adsorption capacity of s-800 for phosphorus was 95mg/g.
Example 3:
placing the dried titanium gypsum and the equivalent amount of paper making sludge in two different porcelain boats respectively, roasting in the same tubular furnace in nitrogen atmosphere at 600 ℃ for 2 hours, naturally cooling to room temperature, placing the titanium gypsum porcelain boats to obtain a product, namely the powdery phosphorus removing agent GS p0 -s-600. Mixing GS p0 Mixing-s-600 with 10wt% of bentonite and 30wt% of water, kneading into clusters, performing extrusion forming, cutting into columnar particles, and drying to obtain the granular phosphorus removal agent PGS p0 -s-600。
30mg of PGS p0 And (4) adding the-s-600 into 30mL of polluted water containing 5-200mg/L of phosphorus to perform a phosphorus static adsorption experiment. The results of the study showed that PGS p0 The saturation adsorption capacity of s-600 for phosphorus was 30mg/g.
Example 4:
mixing the dried titanium gypsum with a proper amount of paper making sludge (2 wt percent), placing the mixture in the same porcelain boat, and placing the porcelain boat in a tube furnace under nitrogen atmosphere 8Roasting at 00 ℃ for 2 hours, naturally cooling to room temperature, and placing the titanium gypsum porcelain boat to obtain a product, namely the powdery phosphorus removal agent GS p2 -800. Mixing GS p2 800, 5 weight percent of carboxymethyl cellulose and 35 weight percent of water are mixed, kneaded into clusters, extruded and molded, cut into columnar particles and dried to prepare the granular phosphorus removal agent PGS p2 -800。
3g of PGS p2 The column adsorption experiment was carried out by loading the column with-800 in a 5mL adsorption column and flowing 5mg/L of contaminated water containing phosphorus through the column at a rate of 1 mL/min. Research results show that the adsorption column can treat about 5L of phosphorus-containing sewage, and the phosphorus content of treated water is lower than 0.5mg/L.
Example 5:
mixing the dried titanium gypsum and a proper amount of paper making sludge (20 wt%), placing the mixture into the same porcelain boat, roasting the mixture for 2 hours at 800 ℃ in a tube furnace in nitrogen atmosphere, naturally cooling the mixture to room temperature, and placing the mixture into the titanium gypsum porcelain boat to obtain a product, namely the powdery phosphorus removal agent GS p20 -800. Mixing GS p20 800, 5wt% of methyl cellulose and 35wt% of water, kneading into a cluster, performing extrusion forming, cutting into columnar particles, and drying to obtain the granular phosphorus removal agent PGS p20 -800。
3g of PGS p20 The column adsorption experiment was carried out by loading the column with-800 in a 5mL adsorption column and flowing 2mg/L of contaminated water containing phosphorus through the column at a rate of 2 mL/min. Research results show that the adsorption column can treat about 15L of phosphorus-containing sewage, and the phosphorus content of the treated water is lower than 0.5mg/L.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The method for preparing the granular phosphorus removing agent by resource utilization of titanium gypsum is characterized by comprising the following steps:
(1) Drying and grinding titanium gypsum waste residues generated in the production process of titanium dioxide to obtain a main raw material G, wherein the titanium gypsum is obtained from the dilute acid neutralization process of titanium dioxide production enterprises, and mainly comprises 60-80wt% of calcium sulfate dihydrate, 10-20wt% of iron oxide, 1-5wt% of titanium oxide and other impurities;
(2) Drying and grinding dewatered sludge generated in the sewage treatment process to obtain an auxiliary raw material S, wherein the dewatered sludge is from a municipal sewage treatment plant, a papermaking sewage treatment plant or an industrial park sewage treatment plant, the solid content is 40-60wt%, and the organic matter content in the solid is 35-55wt%;
(3) Mixing a main raw material G and a proper amount of an auxiliary raw material S, placing the mixture in the same porcelain boat, roasting at a high temperature in a nitrogen atmosphere, drying and grinding to prepare a powdery phosphorus removal agent I; or respectively placing the main raw material G and a proper amount of auxiliary raw material S in different porcelain boats, and roasting, drying, mixing and grinding at high temperature under nitrogen atmosphere to obtain a powdery phosphorus removal agent II, wherein the addition proportion of the auxiliary raw material S is 2-50wt% of the sum of the weight of the main raw material G and the auxiliary raw material S, and the roasting temperature is 600-800 ℃;
(4) Mixing the powdery phosphorus removal agent I or II with a small amount of adhesive and water, kneading into a cluster, extruding and cutting into columnar particles, and drying to obtain the granular phosphorus removal agent, wherein the adhesive is one or more of methylcellulose, carboxymethylcellulose and bentonite, and the addition proportion of the adhesive is 1-10wt% of the weight of the powdery phosphorus removal agent; the diameter of the columnar particles is 1-2mm, the length of the columnar particles is 4-6mm, and the saturated adsorption capacity of the phosphorus removing agent to phosphorus can reach 160mg/g at most.
2. A granular phosphorous removal agent prepared according to the method of claim 1.
3. The application of the granular phosphorous removal agent of claim 2 in the treatment of phosphorus-containing sewage.
4. The use of claim 3, wherein the method of using the phosphorus removal agent comprises directly adding the phosphorus removal agent to the phosphorus-contaminated water body, or packing the phosphorus removal agent into an adsorption column, or using the phosphorus removal agent as an ecological bank protection filler for purifying surface runoff of rivers, reservoirs and lakes.
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| CN114713191A (en) * | 2022-04-18 | 2022-07-08 | 成都理工大学 | Phosphogypsum water body phosphorus removal agent and preparation method and application thereof |
| CN115646444B (en) * | 2022-10-27 | 2024-02-06 | 攀枝花学院 | Sewage dephosphorization material and preparation method thereof |
| CN116173901A (en) * | 2022-12-22 | 2023-05-30 | 济南大学 | Porous biochar prepared from red gypsum and crop straw and application of porous biochar in heavy metal adsorption |
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| CN110526327A (en) * | 2019-09-05 | 2019-12-03 | 郑州大学 | A kind of dephosphorization filler and preparation method thereof |
| CN111943341B (en) * | 2020-08-12 | 2023-01-10 | 中冶一局环境科技有限公司 | Phosphorus removal composition and preparation method thereof, phosphorus removal product and preparation method thereof, and phosphorus removal method |
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