CN101525174B - Compound coagulant made from fly ash and preparation method and application thereof - Google Patents
Compound coagulant made from fly ash and preparation method and application thereof Download PDFInfo
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- CN101525174B CN101525174B CN2009100495412A CN200910049541A CN101525174B CN 101525174 B CN101525174 B CN 101525174B CN 2009100495412 A CN2009100495412 A CN 2009100495412A CN 200910049541 A CN200910049541 A CN 200910049541A CN 101525174 B CN101525174 B CN 101525174B
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Abstract
The invention relates to a compound coagulant made from fly ash and a preparation method and an application thereof. Steps of calcination, activation, acid dipping, alkali dipping, neutralization and copolymerization are used on the fly ash to produce the compound coagulant, that is, an inorganic compound coagulant ingredient of which is polysilicate aluminum ferric sulfate. The compound coagulant makes full use of valuable elements in the fly ash, and has the advantages of simple preparation process, low cost and obvious coagulation effect. No acid wastewater, alkali wastewater or solid waste is discharged, so the preparation method belongs to an advanced environment-friendly clean production process. The obtained compound coagulant is applicable to treatment of urban domestic sewage and industrial wastewater, has strong ability of turbidity removal, color removal and COD removal, and has the advantages of rapid floc forming speed, big and dense floc, rapid sedimentation speed, small sedimented sludge, low treatment cost and the like.
Description
Technical field
The invention belongs to the total utilization of PCA technical field, be specifically related to a kind of compound coagulant of producing with flyash and its production and application
Background technology
Coagulating agent is divided into inorganic coagulant, organic coagulating agent two big classes, and is various in style, its development trend be from low molecule to polymer, by single type to compound, progressively develop to cheap direction practical, non-toxic efficient.Polysilicate class inorganic macromolecular composite coagulating agent is at activated silicic acid and traditional aluminium salt, a kind of new and effective water conditioner that grows up on the coagulating agent bases such as molysite, owing to combine poly-silicic acid bonding, assemble, adsorption bridging usefulness, and the aluminum salt flco is big, good decoloring performance, the iron salt coagulant flco is closely knit, characteristics such as settling velocity is fast, in turbidity removal, decolouring, more similar other kinds in aspect such as removal organism have better effect, in the process water pre-treatment, there is wide application prospect the aspects such as processing of all types of industries waste water and sanitary sewage, and price is suitable, becomes a big research focus of domestic and international inorganic polymer coagulant.
At present in the water treatment procedure most economical easy, widely used be coagulation sedimentation, the quality of its effect often determines operation condition, final outflow water water quality and the cost of subsequent technique flow process, and selecting for use of coagulating agent is the key of decision coagulant precipitation effect quality.Therefore, novel, efficient, low toxicity, multi-functional coagulating agent are the important research development fields of water treatment hi-tech development.
China's flyash quantity discharged is huge, and the efficient high added value recycling of flyash has become the important subject that solution is badly in need of in China.Being rich in the fundamental element of inorganic macromolecular composite coagulating agent in the flyash chemical constitution, is the good raw material of preparation inorganic macromolecular composite coagulating agent.Make full use of the valence component that has in the flyash, preparation composite type inorganic polymer coagulating agent is an effective way of flyash high value added utilization.
Utilize the fly-ash Preparation inorganic polymer coagulant to have problems such as the ferrosilicoaluminum leaching yield is not high at present.
For the flyash production inorganic compounding coagulating agent that utilizes of the present invention, have not yet to see bibliographical information.
Summary of the invention
The present invention proposes that a kind of ferrosilicoaluminum prepares new composite coagulant in the flyash by extracting, and is worth to improve utilization of coal ash, and the treatment of wastes with processes of wastes against one another reduces cost, and overcomes present coagulating agent production and uses the problem that exists in the present situation.
Technical scheme of the present invention
The present invention adopts distinctive roasting, and----in the acidleach--alkali soaks--and unique modern technology of copolymerization, utilize flyash to produce high polymeric composite coagulating agent, products obtained therefrom is actual to be that composition is a kind of inorganic composite type coagulating agent of polysilicate sulfuric acid ferro-aluminum in activation.
The principle of foundation of the present invention
Because the sial in the flyash is with mullite 3Al
2O
32SiO
2Form exists, its SiO
2-Al
2O
3Key bond energy height, the key polymerization degree is big, and chemical property is stable at normal temperatures, and activity is lower, causes the leaching yield of sial lower.With soda and the baking mixed activation of flyash, open SiO
2-Al
2O
3Key makes silicon, aluminium in the flyash change active bigger soluble silicate and unformed body of aluminate or crystal into, thereby improves the leaching yield of sial in the flyash; Mechanical forces such as the friction that produces during ball milling, collision, impact, shearing make particle pulverize, when size reduces, the lattice imperfection, distortion, the degree of crystallinity that cause material reduce even become unformed material, and physical and chemical performance changes, the flyash surface active can be improved, thereby play the mechanical activation effect.
A kind of method of producing compound coagulant with flyash, it comprises the steps:
(1), roasting: under the room temperature, after in container flyash and soda powder being mixed, be warming up to 750 ℃～900 ℃ and carry out roasting, heat-up rate is controlled to be 8 ℃/min～12 ℃/min, and roasting time is 20min～40min; Roasting finishes, and naturally cools to room temperature;
The mass percent that flyash and soda powder mix total amount middle soda powder is 40%～60%;
(2), the activation: with step (1) roasting material with crusher in crushing after, use the ball mill mechanical activation again, rotating speed is 220rpm, material ball ratio is 1: 3, soak time is 2.5h, after sieve;
(3), acidleach: with the flyash grog concentration of step (2) gained is that 2～4mol/L sulphuric acid soln is that 5～25% pulp density carries out acidleach by mass percentage, dissolve the elements such as ferrosilicoaluminum in step (2) the gained flyash grog, extraction time is 2～3h, extraction temperature is a room temperature, and leaching process must be finished under 200r/min stirs; The particle diameter of wherein used flyash grog is less than 0.074mm;
(4), alkali soaks: with the flyash grog concentration of step (2) gained is that 2～4mol/L sodium hydroxide solution is that 5～20% pulp density carries out alkali and soaks by mass percentage, dissolve the elements such as sial in step (2) the gained flyash grog, extraction time is 2～3h, extraction temperature is 70 ℃～90 ℃, and leaching process must be finished under 200r/min stirs;
(5), in and copolymerization: with the alkaline leach liquor of gained in the acid leaching solution of gained in the step (3) and the step (4) is 1: 1～3 to carry out polyreaction at normal temperatures by volume, and polymerization reaction time is 1～24h, promptly gets compound coagulant;
The compound coagulant of final gained is a kind of inorganic composite type coagulating agent of polysilicate sulfuric acid ferro-aluminum among the above-mentioned preparation method, and the amount of substance of (Fe+Al)/Si ratio is 1.5～4.0: 1 in the coagulating agent.
In the method steps (5) of producing compound coagulant with flyash, it is 1: 2.5 by the volume ratio of controlling acid, alkali leaching liquor, assimilation time 12h after the polymerization, resultant (Fe+Al)/Si mol ratio is that 1.72 polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent performance is better.
The composite coagulant that the present invention obtained can be applicable to the processing of city domestic sewage and trade effluent.
Beneficial effect of the present invention
With flyash is main raw material, adopt roasting-activation-acidleach-alkali soak-in and the polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent for preparing of the United Technologies of copolymerization, made full use of the valuable element in the flyash, it is simple, with low cost to have technology, coagulation effect is remarkable, the characteristics that settling of floccus is fast.The no acidic waste water of whole technology, alkaline waste water or solid waste discharge belong to advanced environment-friendly type process for cleanly preparing.
The processing that can be widely used in city domestic sewage and trade effluent with the compound coagulant of flyash production of the present invention, have very strong turbidity removal, remove look, remove the ability of COD, the speed that forms flco is fast, and flco is big and closely knit, settling velocity is fast, and settled sludge volume is little.Use coagulating agent of the present invention can shorten the time of handling waste water, improve the processing power of system, requirement reduces simultaneously, and cost is reduced.
Embodiment
Set forth the present invention with specific embodiment below, but do not limit the present invention.
A kind of method of producing compound coagulant with flyash
Embodiment 1
(1), roasting:
With the Panzhihua Iron power plant fly ash is raw material, and its chemical constitution is as shown in table 1.
Chemical ingredients/the wt% of table 1 raw material powder coal ash
With mass content is that 55% soda powder and flyash mix, and the 300g compound is positioned over roasting in the SX2-10-13 type high temperature retort furnace.Speed with 10 ℃/min at the uniform velocity is warmed up to 850 ℃ from room temperature, is incubated 30min under this maturing temperature.
(2), activation
Behind the furnace cooling, use the palate crusher fragmentation, use ND2-1L type planetary ball mill mechanical activation again, drum's speed of rotation is 220rpm, and material ball ratio is 1: 3, and the mechanical activation time is 2.5h.
Getting particle diameter after the screening is that the following part of 0.074mm is made the leaching raw material in two steps down.
(3), acidleach
Leaching is carried out in SHZ-B type constant temperature water bath vibrator, and sulphuric acid soln concentration is 3mol/L during acidleach, and flyash clinker quality ratio is 5% in the ore pulp, and extraction temperature is 25 ℃, and extraction time is 3h.
(4), alkali soaks
Naoh concentration was 3mol/L when alkali soaked, and pulp density is 5%, and extraction temperature is 80 ℃, and extraction time is 3h.
(5), in and copolymerization
In and copolymerization stage, be 1: 2.5 by volume with the leach liquor of step (3) gained acid leaching liquor and step (4) gained, assimilation time 12h after the polymerization makes (Fe+Al)/Si mol ratio and is controlled to be 1.72 polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent.
Embodiment 2
(1), roasting:
With the Panzhihua Iron power plant fly ash is raw material, and its chemical constitution is shown in the table 1 among the embodiment 1.With mass content is that 55% soda powder and flyash mix, and the 300g compound is positioned over roasting in the SX2-10-13 type high temperature retort furnace.Speed with 10 ℃/min at the uniform velocity is warmed up to 850 ℃ from room temperature, is incubated 30min under this maturing temperature.
(2), activation
Behind the furnace cooling, use the palate crusher fragmentation, use ND2-1L type planetary ball mill mechanical activation again, drum's speed of rotation is 220rpm, and material ball ratio is 1: 3, and the mechanical activation time is 2.5h.
Getting particle diameter after the screening is that the following part of 0.074mm is made the leaching raw material in two steps down.
(3), acidleach
Leaching is carried out in SHZ-B type constant temperature water bath vibrator, and sulphuric acid soln concentration is 3mol/L during acidleach, and flyash clinker quality ratio is 5% in the ore pulp, and extraction temperature is 25 ℃, and extraction time is 3h.
(4), alkali soaks
Naoh concentration was 3mol/L when alkali soaked, and pulp density is 5%, and extraction temperature is 80 ℃, and extraction time is 3h.
(5), in and copolymerization
In and copolymerization stage, be 1: 3 by volume with the leach liquor of step (3) gained acid leaching liquor and step (4) gained, assimilation time 12h after the polymerization makes (Fe+Al)/Si mol ratio and is controlled to be 1.62 polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent.
Embodiment 3
(1), roasting:
With the Panzhihua Iron power plant fly ash is raw material, and its chemical constitution is shown in the table 1 among the embodiment 1.
With mass content is that 55% soda powder and flyash mix, and the 300g compound is positioned over roasting in the SX2-10-13 type high temperature retort furnace.Speed with 10 ℃/min at the uniform velocity is warmed up to 850 ℃ from room temperature, is incubated 30min under this maturing temperature.
(2), activation
Behind the furnace cooling, use the palate crusher fragmentation, use ND2-1L type planetary ball mill mechanical activation again, drum's speed of rotation is 220rpm, and material ball ratio is 1: 3, and the mechanical activation time is 2.5h.
Getting particle diameter after the screening is that the following part of 0.074mm is made the leaching raw material in two steps down.
(3), acidleach
Leaching is carried out in SHZ-B type constant temperature water bath vibrator, and sulphuric acid soln concentration is 3mol/L during acidleach, and flyash clinker quality ratio is 5% in the ore pulp, and extraction temperature is 25 ℃, and extraction time is 3h.
(4), alkali soaks
Naoh concentration was 3mol/L when alkali soaked, and pulp density is 5%, and extraction temperature is 80 ℃, and extraction time is 3h.
(5), in and copolymerization
In and copolymerization stage, be 1: 1 by volume with the leach liquor of step (3) gained acid leaching liquor and step (4) gained, assimilation time 12h after the polymerization makes (Fe+Al)/Si mol ratio and is controlled to be 2.52 polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent.
A kind of application of producing compound coagulant with flyash
Embodiment 4
Synthetic coagulating agent of the present invention is used for simulated wastewater handles, the turbidity of simulated wastewater is 786NTU, and pH is 6.93, and water temperature is 18.2 ℃, and coagulant charging quantity is 10ml/L.The result is as shown in table 2.
Table 2 difference (Fe+Al)/Si coagulating agent flocculating effect contrast
Embodiment 5
The coagulating agent of synthetic of the present invention (Fe+Al)/Si=1.72 is used to handle coke-oven plant, Shanghai City coking industry waste water, and carries out the coagulation effect contrast with commercially available PAC and PFS.Turbidity before the coking industry wastewater treatment is that 36NTU, colourity are that 8 times, COD are 156mL/L.Result is as shown in table 3.
Table 3 Treatment of Coking Effluent result contrast
Embodiment 6
The coagulating agent of synthetic of the present invention (Fe+Al)/Si=1.72 is used to handle Shanghai Baosteel Stainless Steel Branch converter steelmaking sewage, and carries out the coagulation effect contrast with commercially available PAC and PFS.Turbidity before the converter steelmaking sewage disposal is that 2295NTU, colourity are 40 times, and pH is 7.04, and water temperature is 24.6 ℃.Result is as shown in table 4.
Table 4 converter steelmaking sewage disposal result contrast
The result shows, under the identical condition of dosage, the high polymeric composite coagulating agent of flyash polycomponent of the present invention's preparation has very strong turbidity removal ability, remove the look ability, remove the ability of COD, the speed that forms flco is fast, flco is big and closely knit, and settling velocity is fast, and settled sludge volume is little.Use coagulating agent of the present invention can shorten the time of handling waste water, improve the processing power of system, requirement reduces simultaneously, and cost is reduced.
Claims (4)
1. a method of producing compound coagulant with flyash is characterized in that comprising the steps:
(1), roasting: under the room temperature, after in container flyash and soda powder being mixed, be warming up to 750 ℃～900 ℃ and carry out roasting, heat-up rate is controlled to be 8 ℃/min～12 ℃/min, and roasting time is 20min～40min; Roasting finishes, and naturally cools to room temperature;
The mass percent that flyash and soda powder mix total amount middle soda powder is 40%～60%;
(2), the activation: with step (1) roasting material with crusher in crushing after, use the ball mill mechanical activation again, rotating speed is 220rpm, material ball ratio is 1: 3, soak time is 2.5h, after sieve, get particle diameter after the screening and be the following part of 0.074mm and make the leaching raw materials in two steps down;
(3), acidleach: with the flyash grog concentration of step (2) gained is that 2～4mol/L sulphuric acid soln is that 5～25% pulp density carries out acidleach by mass percentage, dissolve the ferrosilicoaluminum element in step (2) the gained flyash grog, extraction time is 2～3h, and extraction temperature is a room temperature;
The particle diameter of wherein used flyash grog is less than 0.074mm;
(4), alkali soaks: with the flyash grog concentration of step (2) gained is that 2～4mol/L sodium hydroxide solution is that 5～20% pulp density carries out alkali and soaks by mass percentage, dissolve the sial element in step (2) the gained flyash grog, extraction time is 2～3h, extraction temperature is 70 ℃～90 ℃, and leaching process must be finished under 200r/min stirs;
(5), in and copolymerization: with the alkaline leach liquor of gained in the acid leaching solution of gained in the step (3) and the step (4) is 1: 1～3 to carry out polyreaction at normal temperatures by volume, and polymerization reaction time is 1～24h, promptly gets compound coagulant.
2. a kind of method of producing compound coagulant with flyash as claimed in claim 1, the compound coagulant that it is characterized in that step (5) gained is a kind of inorganic compounding coagulating agent of polysilicate sulfuric acid ferro-aluminum, and the amount of substance of (Fe+Al)/Si ratio is 1.5～4.0: 1 in the coagulating agent.
3. a kind of method of producing compound coagulant with flyash as claimed in claim 1, it is characterized in that it is 1: 2.5 that passing through in the step (5) controlled the volume ratio of acid, alkali leaching liquor, assimilation time 12h after the polymerization obtains (Fe+Al)/Si mol ratio and is 1.72 polysilicate sulfuric acid ferro-aluminum type inorganic compounding coagulating agent.
4. a kind of method of producing compound coagulant with flyash as claimed in claim 1 is characterized in that the compound coagulant that is obtained can be applicable to the processing of city domestic sewage and trade effluent.
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| CN101525174B true CN101525174B (en) | 2011-06-29 |
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| CN102344171A (en) * | 2010-07-30 | 2012-02-08 | 孙建之 | New method for resource comprehensive utilization of red mud and fly ash |
| CN101948143A (en) * | 2010-10-26 | 2011-01-19 | 山西阳煤丰喜肥业(集团)有限责任公司 | Method for preparing poly-silicate aluminum ferric chloride from fly ash |
| CN103288195A (en) * | 2013-06-28 | 2013-09-11 | 武汉科梦环境工程有限公司 | Method for preparing polysilicate composite coagulant from solid mineral by one-step process |
| CN103395869B (en) * | 2013-07-23 | 2014-11-26 | 内蒙古科技大学 | Water-quenched slag silicate series coagulants and preparation method thereof |
| CN104445541B (en) * | 2013-09-24 | 2016-05-04 | 山东润德净水材料有限公司 | A kind of production method of polysilicate sulfuric acid ferro-aluminum |
| CN103466774A (en) * | 2013-10-10 | 2013-12-25 | 兰州理工大学 | Method for producing compound coagulant by using fly ash |
| CN103864188A (en) * | 2014-03-04 | 2014-06-18 | 长沙理工大学 | Preparation method of inorganic composite flocculant polysilicic acid aluminium ferric chloride |
| CN106348380A (en) * | 2016-09-08 | 2017-01-25 | 北京神雾环境能源科技集团股份有限公司 | Method for preparing water purifying agent by using carbide furnace gas dust |
| CN108083345A (en) * | 2017-12-14 | 2018-05-29 | 中山大学 | A kind of method that polymeric aluminum sulfate silicate iron composite flocculation agent is prepared using red mud waste material |
| CN108557943B (en) * | 2018-04-16 | 2021-04-06 | 广州市芦苇环保科技有限责任公司 | Special water purifying agent for wastewater treatment and preparation method thereof |
| CN109502679B (en) * | 2018-11-19 | 2021-12-31 | 山西大学 | Method for preparing flocculating agent and porous material by synergistic utilization of multiple elements of fly ash |
| CN111204824A (en) * | 2020-01-17 | 2020-05-29 | 广东东日环保股份有限公司 | River surge sewage treatment agent and preparation method thereof |
| CN113072151B (en) * | 2021-04-23 | 2022-05-31 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary polymeric flocculant from vanadium titano-magnetite through one-step method by acid dissolution of hydrochloric acid |
| CN114314788A (en) * | 2022-01-18 | 2022-04-12 | 北京欧亚泉环境投资管理有限公司 | Efficient flocculating agent and preparation method thereof |
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| CN1035623A (en) * | 1989-03-02 | 1989-09-20 | 周天保 | Produce the method for composite flocculation agent with the cinder powder |
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