CN112340827A - Phosphorus removing agent taking acid regeneration silicon-containing mud cake as raw material and preparation method thereof - Google Patents
Phosphorus removing agent taking acid regeneration silicon-containing mud cake as raw material and preparation method thereof Download PDFInfo
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- CN112340827A CN112340827A CN202011043418.2A CN202011043418A CN112340827A CN 112340827 A CN112340827 A CN 112340827A CN 202011043418 A CN202011043418 A CN 202011043418A CN 112340827 A CN112340827 A CN 112340827A
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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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- 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
- C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine compounds
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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
- C02F2101/101—Sulfur compounds
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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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- 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
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/18—PO4-P
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/19—SO4-S
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention provides a phosphorus removing agent taking acid regeneration silicon-containing mud cakes as raw materials and a preparation method thereof, wherein the phosphorus removing agent comprises the following components in parts by weight: 30-50 parts of silicon-containing mud cake, 5-15 parts of silicon-containing mud cake dissolving agent, 10-20 parts of calcium aluminate powder, pH adjusted to 2.0-2.5 by using alkali, 0.05-0.20 part of cationic flocculant and the balance of water. The invention relates to a phosphorus removing agent taking acid regeneration silicon-containing mud cakes as raw materials and a preparation method thereof. On one hand, the resource reuse is realized; on the other hand, the economic cost for treating the phosphorus-containing wastewater is also saved.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a phosphorus removal agent taking acid regeneration silicon-containing mud cakes as a raw material and a preparation method thereof.
Background
The eutrophication of the water body can lead the algae in the water to be rapidly propagated, and the dissolved oxygen in the water is greatly reduced, thereby causing the problems of water quality deterioration, black and odorous water and the like. The overproof forms of various phosphorus discharged into the water body are one of the reasons for causing the eutrophication of the water body, so that the total phosphorus content in the water body is effectively reduced, and the method has very important significance for protecting and restoring the water body. [ CN 101318730A ] discloses a preparation method of an inorganic-organic composite chemical phosphorus removal agent; [ CN 102815778A ] discloses a preparation method of an environment-friendly phosphorus removal agent, which has obvious phosphorus removal effect; the efficient phosphorus removal agent compounded by adopting ferric sulfate, aluminum chloride, poly dimethyl diallyl ammonium chloride and a modifier also has better phosphorus removal effect. Although research on the phosphorus removal agent has made breakthrough progress and achievement, most of the phosphorus removal agent is produced and prepared on the basis of chemical raw materials, and the economic cost is relatively high.
In the industrial production process, various residual resources are generated to be developed and utilized, and the residual resources are utilized in industrial wastewater treatment, so that the treatment of wastes with processes of wastes against one another and the reutilization of resources are better realized.
The hydrochloric acid pickling steel plate is an indispensable part of a cold rolling process, and pickling waste liquid mainly comprises ferrous chloride, excessive hydrochloric acid and a small amount of elemental compounds such as silicon, chromium, manganese, carbon and the like. In order to save resources, the pickling waste liquid is generally recycled, and the common recycling method is acid regeneration to generate regenerated hydrochloric acid which is returned to the pickling section for continuous application; meanwhile, iron in the pickling waste liquid is changed into iron oxide powder which is a main raw material of a ferrite magnetic material. In the acid regeneration process, once elements such as silicon, chromium, manganese, carbon and the like enter the iron oxide powder, the quality of the iron oxide powder is seriously influenced, and particularly, the influence of silicon is most remarkable. To produce high quality iron oxide powders, the spent acid must be desilicated before spray roasting. Desiliconization can be carried out by taking silicon away from waste acid through a certain amount of ferric hydroxide precipitation, a flocculating agent is added in the process to strengthen the sedimentation effect, and finally the desiliconized sludge cake is obtained through pressure filtration by a pressure filter, the desiliconized sludge cake is generally treated and disposed as waste, and how to develop and utilize the desiliconized sludge cake becomes a subject of comprehensive utilization of steel mill resources.
At present, the domestic and foreign sewage and wastewater dephosphorization technology mainly comprises two major types, namely a biological method and a chemical method. Biological phosphorus removal is realized by utilizing microorganisms (phosphorus accumulating bacteria) in activated sludge to release phosphorus and absorb phosphorus, although the operation cost of an operation system of the biological phosphorus removal system is low and the management is convenient, the treatment effect is unstable, the long-time stable standard discharge is difficult to realize, and especially when the concentration of phosphate in inlet water is higher, the treatment effect is more difficult to ensure; the basic principle of chemical phosphorus removal is that phosphate ions in water generate insoluble salt by adding a chemical reagent into wastewater, and the insoluble salt is separated from water after forming a flocculating constituent, so that phosphorus in the wastewater is removed.
Disclosure of Invention
The invention aims to provide a phosphorus removing agent taking acid regeneration silicon-containing mud cakes as raw materials and a preparation method thereof. On one hand, the resource reuse is realized; on the other hand, the economic cost for treating the phosphorus-containing wastewater is also saved.
In order to achieve the purpose, the invention adopts the following technical scheme:
a phosphorus removing agent using acid regeneration silicon-containing mud cakes as raw materials comprises the following components in parts by weight: 30-50 parts of silicon-containing mud cake, 5-15 parts of silicon-containing mud cake dissolving agent, 10-20 parts of calcium aluminate powder, pH adjusted to 2.0-2.5 by using alkali, 0.05-0.20 part of cationic flocculant and the balance of water.
The phosphorus removing agent comprises the following components in parts by weight: 35-45 parts of silicon-containing mud cake, 7-12 parts of silicon-containing mud cake dissolving agent, 13-18 parts of calcium aluminate powder, pH adjusted to 2.0-2.5 by using alkali, 0.10-0.15 part of cationic flocculant and the balance of water.
The silicon-containing mud cake dissolving agent comprises the following components in parts by weight: 8-10 parts of hydrochloric acid, 0.4-0.8 part of ammonium bifluoride, 0.12-0.18 part of sodium gluconate, 0.15-0.2 part of sodium molybdate, 0.04-0.08 part of zinc salt, 0.02-0.05 part of sodium polyacrylate and the balance of water.
The zinc salt is one of zinc chloride, zinc sulfate and zinc nitrate.
The substitute alkali is calcium oxide, Ca (OH)2One or more of active white mud, diatomite, active carbon and saturated alkali solution.
The cationic flocculant is one of poly dimethyl diallyl ammonium chloride, poly dimethylamino ethyl methacrylate and cationic polyacrylamide.
A preparation method of a phosphorus removing agent taking acid regeneration silicon-containing mud cakes as raw materials,
1) preparing a silicon-containing mud cake dissolving agent: adding hydrochloric acid into water, stirring uniformly at a speed of 80-100r/min in a ventilation environment, then respectively adding ammonium bifluoride, sodium gluconate, sodium molybdate, zinc salt and sodium polyacrylate, and stirring uniformly to obtain a silicon-containing mud cake dissolving agent;
2) drying the silicon-containing mud cake at the temperature of 100-110 ℃, grinding the fully dried mud cake in a grinder, sieving with a 200-mesh sieve, taking undersize materials to be fully dissolved in a silicon-containing mud cake dissolving agent, and stirring for 30-60 minutes at the speed of 60-80r/min under a stirrer to obtain homogeneous liquid; adding water into the homogeneous solution, continuously stirring at 40-60r/min, slowly adding calcium aluminate powder into the solution, and stirring for 5-10 min; adjusting the pH value of the liquid to 2.0-2.5 by using substitution alkali; and finally, adding a cationic flocculant (the molecular weight of the cationic polyacrylamide is about 800 under the condition of using the cationic polyacrylamide for preparation, and the use concentration of the cationic polyacrylamide is 0.1 wt% when preparing the phosphorus removing agent) into the obtained solution, and stirring the solution at the speed of 60-100r/min for 30-60 minutes to finally prepare the phosphorus removing agent.
The silicon-containing mud cake is one of the main agents of the complexing agent. The main components of the silicon-containing mud cake are ferric hydroxide and a small amount of silicon dioxide. Drying the silicon-containing mud cake, grinding and sieving with a 200-mesh sieve, taking a certain amount of undersize materials to dissolve in a dissolving agent fully, and stirring at the speed of 60-80r/min under a stirrer to finally obtain a homogeneous liquid, wherein the main component of the liquid is ferric trichloride. Ferric ions can react with phosphate radicals in the wastewater to produce insoluble substances which are then precipitated from the solution. The proportion of the silicon-containing mud cake in the complexing agent is 30-50 parts, preferably 35-45 parts.
The calcium aluminate powder is used as an auxiliary agent, has extremely high activity in an acid environment, can react with phosphate radical in the wastewater, and has an auxiliary effect on a homogeneous liquid silicon-containing mud cake to remove phosphate radical ions more thoroughly; the calcium aluminate powder can effectively remove sulfate radicals and fluoride ions in the wastewater while effectively assisting in removing phosphate radical ions. The proportion of the calcium aluminate powder in the complexing agent is 10-20 parts, preferably 13-18 parts.
The substitute alkali mainly acts as a pH regulator, and the pH regulator of the complexing agent is regulated to a certain range, so that various reactions can be better carried out.
The cationic flocculant is helpful for flocculation and precipitation, so that the factors needing to be treated in water are reduced to the maximum extent. The proportion of the component in the complexing agent is 0.05-0.20 part, preferably 0.10-0.15 part.
Compared with the prior art, the invention has the beneficial effects that:
the phosphorus removal agent is compounded by taking the acid regeneration silicon-containing mud cake as a main component and focusing on a chemical phosphorus removal mechanism, the phosphorus removal agent is used for treating high-concentration phosphorus-containing wastewater, the effect is obvious, and the phosphorus removal rate reaches 89.6%. The phosphorus removing agent has the advantages of low cost, simple preparation method, stable property and obvious effect; meanwhile, the silicon-containing mud cake is reasonably utilized, and the resource reutilization is realized.
1) The main material of the phosphorus removing agent is the acid regeneration silicon-containing mud cake, which belongs to resource recycling and greatly reduces the cost of the composite agent.
2) The phosphorus removing agent disclosed by the invention is easy to obtain all components, good in compounding stability, green, environment-friendly, easily degradable and environment-friendly.
3) The components of the invention have good cooperativity, mutual promotion and stable property; the phosphorus removing agent disclosed by the invention is simple in preparation and use method and easy to operate.
4) The pH range of the complexing agent is wide.
5) The phosphorus removing agent has obvious phosphorus removing effect on high-concentration phosphorus-containing wastewater.
Detailed Description
The present invention will be described in detail with reference to examples, but it should be noted that the practice of the present invention is not limited to the following embodiments.
Example (b):
phosphorus removing agents a, b and c are prepared according to the proportion in the table 1.
Table 1: example phosphorus removing agent a, b and c component proportion
| Ingredients of raw materials | Complexing agent a (portion) | Complexing agent b (portion) | Complexing agent c (portion) |
| Silicon-containing mud cake | 40 | 43 | 37 |
| Silicon-containing mud cake dissolving agent | 10 | 11 | 8 |
| Calcium aluminate powder | 15 | 13 | 17 |
| Substitution alkali | pH value of 2.5 | pH value of 2.5 | pH value of 2.5 |
| Poly dimethyl diallyl ammonium chloride | 0.12 | 0.10 | 0.13 |
| Water (W) | 34.88 | 32.9 | 37.87 |
Example 1:
taking the wastewater of a certain steel plant comprehensive treatment station, wherein the pH value is 8.14, and the SO value is4 2-15mg/L，F-19mg/L total phosphorus was controlled at 69mg/L by phosphate addition. Adding the composite phosphorus removing agents a, b and c into the wastewater in an adding amount of 0.5mL/L, stirring for 10-15 seconds, standing for 60 minutes to determine the total phosphorus content in the supernatant, and obtaining that the total phosphorus is 8.5mg/L, 7.6mg/L and 8.0mg/L respectively; SO (SO)4 2-2.5mg/L, 2.1mg/L and 1.9 mg/L; f-1.8mg/L, 1.7 mg/L.
Example 2:
taking the wastewater of a certain steel plant comprehensive treatment station, controlling the pH to be 8.45, and controlling the total phosphorus to be 35mg/L in a phosphate adding mode. Adding the composite phosphorus removing agents a, b and c into the wastewater in an adding amount of 0.6mL/L, stirring for 10-15 seconds, standing for 60 minutes, and determining the total phosphorus content in the supernatant, thereby obtaining that the total phosphorus is respectively 2.5mg/L, 2.1mg/L and 2.2 mg/L.
Example 3
Taking the wastewater of a certain steel plant comprehensive treatment station, controlling the pH value to be 8.45, and controlling the total phosphorus to be 54.4mg/L in a phosphate adding mode. Adding the composite phosphorus removing agents a, b and c into the wastewater in an adding amount of 0.45mL/L, stirring for 10-15 seconds, standing for 60 minutes, and determining the total phosphorus content in the supernatant, thereby obtaining that the total phosphorus is 3.2mg/L, 3.0mg/L and 3.5mg/L respectively.
Claims (7)
1. A phosphorus removing agent taking acid regeneration silicon-containing mud cakes as raw materials is characterized by comprising the following components in parts by weight: 30-50 parts of silicon-containing mud cake, 5-15 parts of silicon-containing mud cake dissolving agent, 10-20 parts of calcium aluminate powder, pH adjusted to 2.0-2.5 by using alkali, 0.05-0.20 part of cationic flocculant and the balance of water.
2. The phosphorus removal agent taking the acid regeneration siliceous mud cake as the raw material as claimed in claim 1, is characterized in that the phosphorus removal agent comprises the following components in parts by weight: 35-45 parts of silicon-containing mud cake, 7-12 parts of silicon-containing mud cake dissolving agent, 13-18 parts of calcium aluminate powder, pH adjusted to 2.0-2.5 by using alkali, 0.10-0.15 part of cationic flocculant and the balance of water.
3. The phosphorus removing agent taking the acid regeneration siliceous cake as the raw material according to claim 1 or 2, wherein the siliceous cake dissolving agent comprises the following components in parts by weight: 8-10 parts of hydrochloric acid, 0.4-0.8 part of ammonium bifluoride, 0.12-0.18 part of sodium gluconate, 0.15-0.2 part of sodium molybdate, 0.04-0.08 part of zinc salt, 0.02-0.05 part of sodium polyacrylate and the balance of water.
4. The phosphorus removal agent using the acid regeneration silicon-containing mud cake as the raw material as claimed in claim 3, wherein the zinc salt is one of zinc chloride, zinc sulfate and zinc nitrate.
5. The phosphorus removing agent using acid regeneration silicon-containing mud cake as raw material as claimed in claim 1 or 2, wherein the substitute base is calcium oxide, Ca (OH)2One or more of active white mud, diatomite, active carbon and saturated alkali solution.
6. A phosphorus removing agent using acid regeneration silicon-containing mud cake as raw material according to claim 1 or 2, characterized in that the cationic flocculant is one of polydimethyldiallylammonium chloride, polydimethylaminoethyl methacrylate, and cationic polyacrylamide.
7. A process for the preparation of a phosphorus removal agent starting from an acid regenerated silicon-containing sludge cake as claimed in any one of claims 1 to 6,
1) preparing a silicon-containing mud cake dissolving agent: adding hydrochloric acid into water, stirring uniformly at a speed of 80-100r/min in a ventilation environment, then respectively adding ammonium bifluoride, sodium gluconate, sodium molybdate, zinc salt and sodium polyacrylate, and stirring uniformly to obtain a silicon-containing mud cake dissolving agent;
2) drying the silicon-containing mud cake at the temperature of 100-110 ℃, grinding the dried mud cake in a grinder, sieving with a 200-mesh sieve, taking undersize materials to be fully dissolved in a silicon-containing mud cake dissolving agent, and stirring for 30-60 minutes at the speed of 60-80r/min under a stirrer to obtain homogeneous liquid; adding water into the homogeneous solution, continuously stirring at 40-60r/min, slowly adding calcium aluminate powder into the solution, and stirring for 5-10 min; adjusting the pH value of the liquid to 2.0-2.5 by using substitution alkali; and finally, adding a cationic flocculant into the obtained solution, and stirring at the speed of 60-100r/min for 30-60 minutes to finally prepare the phosphorus removing agent.
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| CN202011043418.2A CN112340827A (en) | 2020-09-28 | 2020-09-28 | Phosphorus removing agent taking acid regeneration silicon-containing mud cake as raw material and preparation method thereof |
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| CN202011043418.2A CN112340827A (en) | 2020-09-28 | 2020-09-28 | Phosphorus removing agent taking acid regeneration silicon-containing mud cake as raw material and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815778A (en) * | 2012-08-31 | 2012-12-12 | 广州博芳环保科技有限公司 | Preparation method of environment-friendly phosphorous removing agent |
| CN102863029A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method of using acid regeneration desiliconized mud cakes to prepare superfine iron oxide red |
| CN107399801A (en) * | 2016-05-18 | 2017-11-28 | 东莞市顶盛环保科技有限公司 | Industrial waste water treatment agent based on multiple-effect dephosphorization |
| WO2018169395A1 (en) * | 2017-03-15 | 2018-09-20 | Stichting Wetsus, European Centre Of Excellence For Sustainable Water Technology | Method and system for phosphate recovery from a stream |
| CN108914133A (en) * | 2018-08-15 | 2018-11-30 | 鞍钢贝克吉利尼水处理有限公司 | Cleaning agent and application method for cold-rolling pickling regeneration unit eliminating sludge in pipe |
-
2020
- 2020-09-28 CN CN202011043418.2A patent/CN112340827A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102815778A (en) * | 2012-08-31 | 2012-12-12 | 广州博芳环保科技有限公司 | Preparation method of environment-friendly phosphorous removing agent |
| CN102863029A (en) * | 2012-09-25 | 2013-01-09 | 上海应用技术学院 | Method of using acid regeneration desiliconized mud cakes to prepare superfine iron oxide red |
| CN107399801A (en) * | 2016-05-18 | 2017-11-28 | 东莞市顶盛环保科技有限公司 | Industrial waste water treatment agent based on multiple-effect dephosphorization |
| WO2018169395A1 (en) * | 2017-03-15 | 2018-09-20 | Stichting Wetsus, European Centre Of Excellence For Sustainable Water Technology | Method and system for phosphate recovery from a stream |
| CN108914133A (en) * | 2018-08-15 | 2018-11-30 | 鞍钢贝克吉利尼水处理有限公司 | Cleaning agent and application method for cold-rolling pickling regeneration unit eliminating sludge in pipe |
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Application publication date: 20210209 |