CN101830477B - Technology for preparing PSAF (Polymer Silica Aluminum Ferrum) by waste rock base raw material - Google Patents
Technology for preparing PSAF (Polymer Silica Aluminum Ferrum) by waste rock base raw material Download PDFInfo
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- CN101830477B CN101830477B CN 201010197036 CN201010197036A CN101830477B CN 101830477 B CN101830477 B CN 101830477B CN 201010197036 CN201010197036 CN 201010197036 CN 201010197036 A CN201010197036 A CN 201010197036A CN 101830477 B CN101830477 B CN 101830477B
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Abstract
The invention discloses a technology for preparing PSAF (Polymer Silica Aluminum Ferrum) by a waste rock base raw material. The inorganic polymer flocculant-PSAF is mainly prepared from waste rock base materials by the synthesis process comprising the steps of active waste rock base raw material preparation, alkali extraction under heating and pressurizing condition, acid extraction under heating and pressurizing condition and slow concentration polymerization under heating condition. The PSAF flocculant prepared by the technology is a tawny semisolid substance, wherein the content of silica is 20-30 percent, the content of aluminum is 15-21 percent and the content of ferrum is 6-15 percent. Compared with the prior art, the invention simplifies technology, saves energy, has high extraction efficiency and can prepare the PSAF flocculant with good degree of polymerization, high treatment efficiency and level and small dosage in water treatment compared with the PSAF flocculant prepared by the conventional method.
Description
[technical field]
The present invention relates to a kind of preparation technology of material and according to the material of this prepared gained, the process method that particularly preparation gathers the ferrosilicoaluminum flocculation agent from coal gangue or flyash, and gather the ferrosilicoaluminum flocculation agent with what this prepared went out.
[background technology]
In recent years; In energy dilemma and crisis of resource day by day under the serious situation; Utilizing the higher useful element of content in the waste, is the feedstock production coagulant with the trade waste, and making full use of exploitable resources is one of main trends of world today's coagulating agent researchdevelopment.Turn waste into wealth, the treatment of wastes with processes of wastes against one another is environmental improvement and the most promising developing direction of refuse renewable resources.The spoil based raw material mainly comprises coal gangue and flyash.China is the maximum coal mining state in the whole world, is brought to the coal gangue on ground with the exploitation of coal, become maximum solid waste source, so the comprehensive treating process of coal gangue has become, and people pays special attention to and problem demanding prompt solution.Contain elements such as a large amount of iron, silicon, aluminium in the coal gangue, utilize its synthesizing inorganic flocculation agent to cause people's research enthusiasm greatly in recent years.And flyash is through the product behind the power plant high temperature sintering, and wherein silicon, aluminium, ferro element can strippings, and therefore utilizing the various flocculation agents of fly-ash Preparation also is a research focus in flocculation agent field in recent years.
Comprise mainly in the active silicic acid metallic salt flocculation agent and gather ferrosilicoaluminum, gather sial and ferric-polysilicate that the three relatively gathers ferrosilicoaluminum and on flocculating effect, more takes advantage.
At present, spoil based raw material preparation of industrialization both at home and abroad gathers the compound method that silicon gathers the ferrosilicoaluminum flocculation agent and mainly contains:
1, polymeric ferric aluminum joins to form in the polymeric silicicacid for preparing and gathers ferrosilicoaluminum: State Intellectual Property Office's Granted publication on July 26th, 2006; Disclosed a kind of synthesis technique in the patent of invention of Granted publication CN 1266038C " compound method of gathering ferrosilicoaluminum "; This technology joins the ferric sulfate of preparation in the flyash acid extract, at solid Na
2CO
3Leave standstill the back under the stirring condition and form polymeric ferric aluminum, continue join to form in the polymeric silicicacid for preparing gathered the ferrosilicoaluminum finished product.This kind preparation method will use a large amount of iron content starting material, and preparation technology is loaded down with trivial details, drawn to gather ferrosilicoaluminum flocculant poly degree lower, processing efficiency and processing horizontal are limited.Need to flyash acvator participate in down through high-temperature roasting (800～850 ℃, 4～12h), with stripping its siliceous, aluminium, ferro element, the required energy is bigger.
2, add molysite behind the preparation aluminium silicate polymer and obtain gathering the ferrosilicoaluminum flocculation agent: the spoil based raw material prepares the technology of aluminium silicate polymer; The application number of announcing on January 16th, 2008 like State Intellectual Property Office is a disclosed process step " process method for preparing active carbon-oxide composite absorbing material from coal gangue and gather sial " application for a patent for invention of CN 200710137852.5, and this process step comprises that gangue ingredient, activation, alkali are put forward the activation reflux, activation reflux, washing oven dry, normal temperature slaking, drying are put forward in acid.But this kind technology can only be extracted silicon, aluminium composition in the coal gangue, and extraction efficiency is low, as obtaining gathering the ferrosilicoaluminum flocculation agent, also needs extra adding molysite, increases preparation cost.And this kind technology needs twice reflux, and water resource waste is huge.
[summary of the invention]
Technical assignment of the present invention is the deficiency to above prior art, and the technology that preparation gathers ferrosilicoaluminum in a kind of spoil based raw material is provided, and this kind technology can directly prepare from the spoil based raw material and gather ferrosilicoaluminum, and saves resources such as water, heating power.
The technical scheme that the present invention solves its technical problem is:
The technology that a kind of spoil based raw material preparation gathers ferrosilicoaluminum; It is characterized in that: with spoil base material is that main raw material prepares inorganic polymer flocculant---gather ferrosilicoaluminum; In building-up process; Take under the heating and pressurizing that alkali is carried, acid is carried under the heating and pressurizing, heating state slowly concentrates polymerization down, its concrete process step is following:
(1) gets the raw materials ready: active spoil based raw material;
(2) alkali is carried under the heating and pressurizing: in the activated feedstock of step 1, add 15%～30%NaOH solution, with coal gangue fine powder solvent and solute weight ratio be that 2:1 is to 6:1; Reaction times 2h, 100 ℃～150 ℃ of temperature, pressure is 5 MPas～10 MPas, solid-liquid separation, the filtrating of collection is the alkali extract;
(3) acid is carried under the heating and pressurizing: in the filter residue of step 2, add the inorganic acid solution of 10%～20% concentration, solvent and solute weight ratio is that 2:1 is to 6:1; Reaction times 2h, 100 ℃～150 ℃ of temperature, pressure is 5 MPas～10 MPas, solid-liquid separation, the filtrating of collection is sour extract, and the volume of adjustment gained acid extract is equal to step 2 gained alkali extract;
(4) heating state slowly concentrates polymerization down: step 3 gained acid extract is dropwise joined in the step 2 gained alkali extract, and the volume ratio of said sour extract and alkali extract is that 1:1 is to 2:1; 70 ℃～100 ℃ of temperature of reaction leave standstill and wait to obtain the tawny semi-solid material.
Inorganic acid solution in the above-mentioned steps 3 is meant the mixing acid of hydrochloric acid, vitriolic any one or arbitrary proportion.
The adjustment pH value of solution is 3～4 in the above-mentioned steps 4.
Spoil base activated feedstock in the above-mentioned steps 1 is a flyash.
Spoil base activated feedstock preparation technology in the above-mentioned steps 1 is: the colliery powder comminution is thin, and the adding activator mix is even, and above-mentioned compound is added thermal bake-out for 600 ℃～800 ℃, is incubated 1 hour and gets spoil base activated feedstock.
Above-mentioned acvator is Na
2CO
3, with coal gangue fine powder part by weight be 3:4.
Above-mentioned acvator is CaCO
3, with coal gangue fine powder part by weight be 3:4.
Above-mentioned acvator is the CaCO of 1:1 mixed
3With NaOH, mixture and coal gangue fine powder part by weight are 3:4.
The preparation of the spoil based raw material of claim 1 gathers that the technology of ferrosilicoaluminum is prepared to go out to gather the ferrosilicoaluminum flocculation agent, it is characterized in that being the tawny semi-solid material, and wherein silicone content is 20%～30%, and aluminium content is 15%～21%, iron level is 6%～15%.
Compared with prior art, the present invention has the following advantages:
1, starting material are single, need not to add other iron content starting material, practice thrift cost;
2, heating, the technology that pressurization alkali dissolves and heating, pressurization acid are dissolved have improved spoil based raw material silicon, aluminium, ferro element extraction efficiency, have improved the quality of product;
3, need not reflux, save water resources, simplify technology, make it more appropriate to suitability for industrialized production;
4, dropwise mix under the heating state, slowly slaking, concentrating the polymerization gained, to gather ferrosilicoaluminum flocculant poly degree good, and processing efficiency and processing horizontal are high, and the water treatment dosage is gathered the ferrosilicoaluminum flocculation agent less than the ordinary method preparation.
[embodiment]
It is following that traditional technology utilizes coal gangue or fly-ash Preparation to gather the process flow steps of ferrosilicoaluminum flocculation agent:
(1) get the raw materials ready: flyash or pulverising mill duff spoil add 1.5 times Na
2CO
3Powder;
(2) activation: add thermal bake-out with above-mentioned material 600-850 ℃, be incubated 4 hours spoil base activated feedstock;
(3) alkali is carried: in the activated material of step 2, add 15%NaOH solution, with the material solvent and solute weight ratio be 5:1; Reaction times 2h, 100 ℃ of temperature, reflux 2h under the normal pressure, suction filtration, the filtrating of collection is the alkali extract;
(4) acid is carried: in the filter residue of step 3, add 15%HCl solution, solvent and solute weight ratio is 5:1; Reaction times 2h, 100 ℃ of temperature, reflux 2h under the normal pressure, suction filtration, the filtrating of collection is sour extract;
(5) add an amount of ferric sulfate according to required processing wastewater property;
(6) slaking: step 4 gained acid extract is joined in the step 3 gained alkali extract, and the volume ratio of sour extract and alkali extract is 1:1; The temperature remains within the normal range, leaves standstill to wait to obtain pale brown look liquid.
Embodiments of the invention 1 utilize the coal gangue preparation to gather the ferrosilicoaluminum flocculation agent, and concrete steps are following:
(1) batching: the spoil based raw material is coal gangue 15g, pulverizes levigate, the adding and the CaCO of volume of material than 3:4
3Mix;
(2) activation: above-mentioned material is added thermal bake-out for 600 ℃, be incubated 1 hour and get spoil base activated feedstock;
(3) alkali is carried under the heating and pressurizing: in the activated material of step 2, add 15%NaOH solution, with coal gangue fine powder solvent and solute weight ratio be 2:1; Reaction times 2h, 100 ℃ of temperature, pressure 5 MPas, solid-liquid separation, the filtrating of collection is the alkali extract;
(4) acid is carried under the heating and pressurizing: in the filter residue of step 3, add 10%HCl solution, solvent and solute weight ratio is 2:1; Reaction times 2h, 100 ℃ of temperature, pressure 5 MPas, solid-liquid separation, the filtrating of collection is sour extract, and the volume of adjustment gained acid extract is equal to step 3 gained alkali extract;
(5) heating state slowly concentrates polymerization down: step 4 gained acid extract is dropwise joined in the step 3 gained alkali extract, and the volume ratio of said sour extract and alkali extract is 1:1; 70 ℃ of temperature of reaction, the adjustment pH value of solution is 3～4, obtains the tawny semisolid after leaving standstill 2h.
Use CaCO in this kind process program
3Activation, cost value is cheap, and sedimentation is fast.
The embodiment of the invention 2 utilizes the coal gangue preparation to gather the ferrosilicoaluminum flocculation agent, and wherein, the adding acvator is and the Na of volume of material than 3:4 in the step 1
2CO
3The heating maturing temperature is 800 ℃; The NaOH strength of solution is 30%, and the HCl strength of solution is 20%, and the solvent and solute weight ratio that acid is carried, alkali is carried middle soda acid and coal gangue fine powder is 6:1; 150 ℃ of temperature, pressure 10 MPas; The sour extract and the volume ratio of alkali extract that concentrate in the polymerization procedure are 2:1, and 100 ℃ of temperature of reaction obtain the tawny semisolid after leaving standstill 2h.All the other parameter steps are with embodiment 1.
The embodiment of the invention 3 utilizes the coal gangue preparation to gather the ferrosilicoaluminum flocculation agent, and wherein, the adding acvator is and the CaCO of volume of material than the 1:1 mixed of 3:4 in the step 1
3With NaOH; The heating maturing temperature is 700 ℃; The NaOH strength of solution is 20%, H
2SO
4Strength of solution is 15%, and the solvent and solute weight ratio that acid is carried, alkali is carried middle soda acid and coal gangue fine powder is 4:1; 120 ℃ of temperature, pressure 8 MPas; The sour extract and the volume ratio of alkali extract that concentrate in the polymerization procedure are 1.5:1, and 80 ℃ of temperature of reaction obtain the tawny semisolid after leaving standstill 2h.All the other parameter steps are with embodiment 1.
Technology described in the embodiment 1～3, coal gangue be under the raw material heating and pressurizing alkali carry with heating and pressurizing under acid carry than traditional technology silicon extraction yield and improve 5～11.5%, it is about 9～17% that the aluminium extraction yield improves, the iron extraction yield improves 4～5%.
And avoided reflux, saved the waste of water resources.
Need 600～850 ℃ of high-temperature roastings in the traditional technology in the reactivation process; Insulation 4～12h, disclosed technology adds thermal bake-out for 600 ℃～800 ℃ among the present invention, be incubated 1 hour and get final product spoil base activated feedstock; The energy that uses has obtained saving, meets the environmental requirement of energy-saving and emission-reduction.
The embodiment of the invention 4: utilize fly-ash Preparation to gather the ferrosilicoaluminum flocculation agent, concrete steps are following:
(1) batching: the spoil based raw material is flyash 15g;
(2) alkali is carried under the heating and pressurizing: in the activated material of step 2, add 20%NaOH solution, with coal gangue fine powder solvent and solute weight ratio be 4:1; Reaction times 2h, 120 ℃ of temperature, pressure 8 MPas, solid-liquid separation, the filtrating of collection is the alkali extract;
(3) activation is proposed in acid under the heating and pressurizing: in the filter residue of step 3, add 15%HCl solution, solvent and solute weight ratio is 2:1; Reaction times 2h, 120 ℃ of temperature, pressure 8 MPas, solid-liquid separation, the filtrating of collection is sour extract, and the volume of adjustment gained acid extract is equal to step 2 gained alkali extract;
(4) heating state slowly concentrates polymerization down: step 4 gained acid extract is dropwise joined in the step 3 gained alkali extract, and the volume ratio of sour extract and alkali extract is 1:1; 80 ℃ of temperature of reaction, the adjustment pH value of solution is 3～4, obtains the tawny semi-solid material after leaving standstill 2h.
It is auxiliary that this kind technology, flyash need not acvator, and omitted the step of high-temperature roasting, and the cost and the energy save material.Simplified preparation technology, be more suitable in suitability for industrialized production.
The embodiment of the invention 5: utilize fly-ash Preparation to gather the ferrosilicoaluminum flocculation agent, wherein, the two-step acid-alkali reaction conditions is: solvent and solute weight ratio is 2:1; 100 ℃ of temperature, pressure 5 MPas.Concentrate 70 ℃ of polymeric reaction temperatures, obtain the tawny semi-solid material after leaving standstill 2h.All the other are with embodiment 4.
The embodiment of the invention 6: utilize fly-ash Preparation to gather the ferrosilicoaluminum flocculation agent, wherein, the two-step acid-alkali reaction conditions is: solvent and solute weight ratio is 6:1; 150 ℃ of temperature, pressure 10 MPas.Concentrate 100 ℃ of polymeric reaction temperatures, obtain the tawny semi-solid material after leaving standstill 2h.All the other are with embodiment 4.
Embodiment 4～6 said technologies, flyash be under the raw material heating and pressurizing alkali carry with heating and pressurizing under acid carry than traditional technology silicon extraction yield and improve 5.5～11.2%, it is about 8.7～16.2% that the aluminium extraction yield improves, the iron extraction yield improves 4.4～5.4%.
The ferrosilicoaluminum flocculation agent that gathers of above embodiment preparation technology gained is the tawny semi-solid material, and wherein silicone content is 20%～30%, and aluminium content is 15%～21%, iron level is 6%～15%
In the above-mentioned technology, sour extract is dropwise added in the alkali extract, and the mixed solution of soda acid extracting solution is carried out slowly concentrating polymerization; Resultant tawny semi-solid gathers the ferrosilicoaluminum flocculation agent; Make its polymerization more abundant, promptly increased its polymerization degree, improved flocculation agent processing efficiency and processing horizontal.
High-COD waste water is handled experimental result and is shown, handles 5ml Shengli Oil Field well-drilling waste water and need add by 1.25% of 10g coal gangue gained flocculation dosage, adds 0.3% of same amount coal gangue products obtained therefrom through needing after the process modification, and dosage reduces about 76%.
The flco degree of compactness that forms in the processing Shengli Oil Field well-drilling waste water gained system is far above the degree of compactness of the flco that forms in the system before not optimizing.Wherein the ferrosilicoaluminum polymerization state is best for the ferrosilicoaluminum flocculation agent that gathers of disclosed prepared among process the present invention, and flocculation ability strengthens.The flocculation agent of producing with traditional technology compares, and its difference is in the flocculation agent existence different, and the ferrosilicoaluminum polymerization state also can change to some extent, so the flocculation agent ability is also inequality.
What waste water added disclosed prepared among the present invention gathers the ferrosilicoaluminum flocculation agent, forms flco and is suspended in clarification upper strata at night, and flco also is not destroyed behind the turned upside down container 10 times, and subnatant is still clarified.Form settling of floccus in the bottom of system and adopt the traditional technology gained to gather the ferrosilicoaluminum flocculation agent, inverted container once, flco promptly disperses again, it is muddy that system becomes.Explain that the ferrosilicoaluminum flocculant poly degree that gathers of disclosed prepared increases among the present invention, significantly improved its processing efficiency and processing horizontal.
Claims (8)
1. a spoil based raw material prepares the method for gathering ferrosilicoaluminum; It is characterized in that: with spoil base material is main raw material; The preparation inorganic polymer flocculant---gather ferrosilicoaluminum; In building-up process, take under the heating and pressurizing that alkali is carried, acid is carried under the heating and pressurizing, heating state slowly concentrates polymerization down, its concrete grammar step is following:
(1) gets the raw materials ready: active spoil based raw material;
(2) alkali is carried under the heating and pressurizing: in the activated feedstock of step 1, be incorporated as 15% ~ 30% NaOH solution, with coal gangue fine powder solvent and solute weight ratio be that 2:1 is to 6:1; Reaction times 2h, 100 ℃ ~ 150 ℃ of temperature, pressure is 5 MPas ~ 10 MPas, solid-liquid separation, the filtrating of collection is the alkali extract;
(3) acid is carried under the heating and pressurizing: in the filter residue of step 2, be incorporated as the inorganic acid solution of 10% ~ 20% concentration, solvent and solute weight ratio is that 2:1 is to 6:1; Reaction times 2h, 100 ℃ ~ 150 ℃ of temperature, pressure is 5 MPas ~ 10 MPas, solid-liquid separation, the filtrating of collection is sour extract, and the volume of adjustment gained acid extract is equal to step 2 gained alkali extract;
(4) heating state slowly concentrates polymerization down: step 3 gained acid extract is dropwise joined in the step 2 gained alkali extract, and the volume ratio of said sour extract and alkali extract is that 1:1 is to 2:1; 70 ℃ ~ 100 ℃ of temperature of reaction leave standstill and wait to obtain the tawny semi-solid material.
2. the method that spoil based raw material according to claim 1 preparation gathers ferrosilicoaluminum is characterized in that inorganic acid solution in the said step 3 is meant the mixing acid of hydrochloric acid, vitriolic any one or arbitrary proportion.
3. the method that spoil based raw material preparation according to claim 1 gathers ferrosilicoaluminum is characterized in that the adjustment pH value of solution is 3 ~ 4 in the said step 4.
4. the method that spoil based raw material preparation according to claim 1 gathers ferrosilicoaluminum is characterized in that the active spoil based raw material in the said step 1 is a flyash.
5. the method that spoil based raw material preparation according to claim 1 gathers ferrosilicoaluminum; It is characterized in that the active spoil based raw material preparation method in the said step 1 is: the colliery powder comminution is thin; It is even to add activator mix; Above-mentioned compound is added thermal bake-out for 600 ℃ ~ 800 ℃, be incubated 1 hour and get spoil base activated feedstock.
6. the method that spoil based raw material preparation according to claim 5 gathers ferrosilicoaluminum is characterized in that said acvator is Na
2CO
3, with coal gangue fine powder part by weight be 3:4.
7. the method that spoil based raw material preparation according to claim 5 gathers ferrosilicoaluminum is characterized in that said acvator is CaCO
3, with coal gangue fine powder part by weight be 3:4.
8. the method that spoil based raw material preparation according to claim 5 gathers ferrosilicoaluminum is characterized in that said acvator is the CaCO of 1:1 mixed
3With NaOH, mixture and coal gangue fine powder part by weight are 3:4.
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| CN101955232B (en) * | 2010-09-30 | 2012-04-18 | 济南大学 | Poly silicate ferric aluminum chloride (PSFAC) coagulant prepared from grain slag |
| CN101948142A (en) * | 2010-10-09 | 2011-01-19 | 天津泰达环保有限公司 | Method for producing sludge modifier by utilizing coal gangue |
| CN102452655B (en) * | 2010-10-29 | 2015-04-08 | 淮南师范学院 | Method for simultaneously preparing poly aluminum-ferric-silicate flocculant and low silicon X type molecular sieve |
| CN103991940B (en) * | 2011-03-29 | 2016-02-03 | 济宁医学院 | A kind of coal ash for manufacturing is for hybrid flocculant technique |
| CN102531328A (en) * | 2012-01-09 | 2012-07-04 | 济南大学 | Composite inorganic polymeric sludge dehydration conditioner prepared from blast-furnace metallurgical slag |
| 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 |
| CN105692831A (en) * | 2016-02-26 | 2016-06-22 | 武汉理工大学 | Efficient slag-based inorganic phosphorous removal flocculating agent and preparation method thereof |
| CN106315603A (en) * | 2016-08-04 | 2017-01-11 | 广东紫方环保技术有限公司 | Preparation method of polymeric aluminum ferric silicate |
| CN109809540B (en) * | 2017-11-20 | 2021-11-05 | 临沂大学 | Polysilicate aluminum ferric flocculant and preparation method thereof |
| CN109809419B (en) * | 2017-11-20 | 2022-06-14 | 临沂大学 | Method for preparing polysilicate aluminum ferric flocculant |
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| CN1325391C (en) * | 2006-03-17 | 2007-07-11 | 重庆市化工研究院 | Method of producing poly aluminium iron silicate composite flocculating agent using fly ash and ferrous sulphate |
| CN100577579C (en) * | 2007-08-24 | 2010-01-06 | 中国石油大学(华东) | Method for producing water treatment coagulant by using coal gangue |
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