CN109319896A - The method for preparing flocculant with flyash and vanadium titano-magnetite - Google Patents
The method for preparing flocculant with flyash and vanadium titano-magnetite Download PDFInfo
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- CN109319896A CN109319896A CN201811307793.6A CN201811307793A CN109319896A CN 109319896 A CN109319896 A CN 109319896A CN 201811307793 A CN201811307793 A CN 201811307793A CN 109319896 A CN109319896 A CN 109319896A
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- magnetite
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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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
- C02F2101/20—Heavy metals or heavy metal 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
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to waste utilization technical fields, and in particular to a method of flocculant is prepared with flyash and vanadium titano-magnetite.For existing long, at high cost for the method flow of flocculant using coal ash for manufacturing, the problem of flocculating effect difference, the present invention provides a kind of methods for preparing flocculant with flyash and vanadium titano-magnetite, and steps are as follows: a, vanadium titano-magnetite is crushed, it is spare；B, vanadium titano-magnetite is taken, is dissolved in NaOH solution, 60~90min is reacted, takes supernatant liquor A；C, flyash is taken, HCl and H that volume ratio is 1~3 ︰ 1 is added2SO4, NaCl is added, 0.5~2.5h of temperature constant magnetic stirring at 25~35 DEG C obtains the mixture of fly ash of sour processing, takes supernatant liquor B；D, by A liquid and B liquid, 1~5 ︰ 1 is mixed by volume, then the evaporative crystallization at 80~150 DEG C, obtains polysilicate flocculant.The advantages of present invention is prepared for a kind of polysilicate flocculant, combines aluminium system and iron-based flocculating agent, flocculating effect is good；Preparation flow is simple, at low cost.
Description
Technical field
The invention belongs to solid waste to utilize technical field, and in particular to a kind of to be prepared with flyash and vanadium titano-magnetite
The method of flocculant.
Background technique
Flocculant be refer to generate floccule, and can by absorption, gantry, be crosslinked the effects of make it is insoluble in solution
One substance of substance, colloid or suspended particle removal.It mainly include natural flocculating agent, inorganic polymer flocculant is organic
Synthetic polymeric flocculant and microbial flocculant etc..Inorganic flocculating agent mainly includes silicate, aluminium salt, molysite and its hydrolysis
Polymer etc., it is from a wealth of sources, it is simple process, nontoxic, cheap, better than biology effect in wastewater treatment and eutrophication problem
It answers, thus in the actual production process, inorganic flocculating agent is using more.
The solid waste flyash that coal-fired power plant generates in power generation process, main component SiO2And Al2O3Account for about it
The 57%~95% of total weight.2015,6.3 hundred million tons of China's common property fecula coal ash, it is contemplated that be up to 9.2 hundred million tons to the year two thousand twenty.
If flyash can be fully used, not only vast resources can also be saved with environment purification.From the more macromolecule of early stage
The coagulant polysilicate of quality arrives polymerization Al, Si, Fe polymer and various composite type inorganic polymer flocculants, it
Be still current research and application hot spot.Using rich in Al, Si, Fe waste minerals resource (such as flyash, gangue,
Pyrite cinder etc.) composite coagulant flocculant is produced, it not only reduced costs, but also waste can be comprehensively utilized, had
Biggish social effect and economic benefit.
In order to make full use of flyash, coal ash for manufacturing can be used for flocculant.
As patent CN107934978A discloses a kind of coal ash for manufacturing for the method for inorganic polymer flocculant, using flyash
Alkalinity calcination, sodium hydroxide solution leaching separation SiO2And Al, leachate are acidified tone pitch, isolated aluminium silicate polymer, hydroxide
Sodium solution leaching slag acidleach, pickle liquor are concentrated by evaporation, and tone pitch, polymerization obtains ferric sulfate liquid product.
Patent CN103408117A discloses a kind of simple and easy method using flyash production poly silicate aluminium ferric flocculating agent, presses
Solid is added to flyash than 1.2 according to sode ash, with 750 DEG C of roasting 1.5h in Muffle furnace after ground and mixed is uniform, blowing out is natural
It is spare after cooling.2mol/LHCl is selected, to carry out acidleach to product of roasting under liquid-solid ratio 15mL/g room temperature, stirring and dissolving is (without surplus
Remaining residue), it can get H2SiO3, aluminium chloride and chlorination iron mixed solution.Adjust leachate Si:Al (mol:mol) be 1:0.4,
Si:Fe (mol:mol) be 1:0.8, pH value 1.5, it is ripe controlled at 50 DEG C in the reaction kettle with polytetrafluoroethyllining lining
Change 2h up to liquid poly silicate aluminium ferric flocculating agent, solid product can be obtained after 40 DEG C dry.
Patent CN101182061A discloses a kind of flyash and kaolin production highly-effective compound polysilicate aluminum iron flocculation
The method of agent, in 50~120 degree celsius temperature items after flyash, kaolin, quick lime and water are sufficiently mixed by a certain percentage
It heats 4~8 hours under part and is filtered after natural cooling, filtrate tune pH value to 6~10 obtains filtrate I；Concentration is added in gained filter residue is
36.7% technical hydrochloric acid is heated 4~8 hours under the conditions of 50~120 degree celsius temperature after mixing and is filtered after natural cooling, is obtained
Filtrate II；1:1 is mixed by volume for filtrate I and filtrate II, stirring, tune pH value to 3~5, is obtained prepared by the present invention after standing
Liquid product.
Above-mentioned is mostly first to calcine, then acidleach or alkali soak for the technology of flocculant using coal ash for manufacturing, and operating process is longer, and
The risk and cost is relatively high.
Low-grade vanadium titano-magnetite refers mainly to grade between cutoff grade (20%) and production-grade (25%), is arranged
For the ore that industrially cannot be temporarily utilized, essential mineral composition has ilmenite, titanomagnetite, pyroxene, plagioclase, hornblend
With olivine etc..Increasingly sharpen as scarcity of resources is contradictory, comprehensive reutilization low-grade vanadium titano-magnetite still becomes must
So.Composite coagulant flocculant is produced using low-grade vanadium titano-magnetite, comprehensively utilizes waste, there is biggish society
Meaning and economic benefit.Also a new thinking is provided for low-grade vanadium titano-magnetite comprehensive utilization, there is no to look at present and uses vanadium
Titanomagnetite produces the precedent of flocculant.
Summary of the invention
The technical problem to be solved in the present invention are as follows: it is existing long, at high cost for the method flow of flocculant using coal ash for manufacturing,
Flocculating effect problem to be improved.
The technical solution of present invention solution above-mentioned technical problem are as follows: a kind of flyash and vanadium titano-magnetite preparation wadding are provided
The method of solidifying agent.Method includes the following steps:
A, vanadium titano-magnetite is crushed, it is spare；
B, the vanadium titano-magnetite for taking step a to obtain, is dissolved in NaOH solution, reacts 60~90min, takes supernatant liquor A；
C, flyash is taken, HCl and H that volume ratio is 1~3 ︰ 1 is added2SO4, NaCl is added, the constant temperature at 25~35 DEG C
0.5~2.5h of magnetic agitation obtains the mixture of fly ash of sour processing, takes supernatant liquor B；
D, by A liquid and B liquid, 1~5 ︰ 1 is mixed by volume, then the evaporative crystallization at 80~150 DEG C, obtains polysilicate wadding
Solidifying agent.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, magnetic iron ore described in step a is
The low-grade vanadium titano-magnetite of TFe content≤25%.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, smashed granularity described in step a
To cross 160~200 meshes.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, low grade vanadium titanium magnetic described in step b
The weight ratio of iron ore and NaOH are as follows: 3~6 ︰ 30~50.
Further, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, the NaOH solution is dense
Degree is 25~40%.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, cosolvent NaCl described in step c
Additional amount are as follows: NaCl1~4g is added in every 40~60g flyash.
The invention has the benefit that
The present invention provides a kind of methods for preparing flocculant with flyash and low-grade vanadium titano-magnetite, useless using solid
Gurry flyash and low-grade vanadium titano-magnetite prepare polysilicate using the effect of highly basic and mixed acid and flocculate at normal temperature
Agent.The advantages of polysilicate flocculant is the compound of polysilicon acid and metal salt, combines aluminium system and iron-based flocculating agent, and subtract
Weak mutual weakness not only has adsorption bridging effect and charge neutrality effect, but also the big, Multicomponent phase with molecule aggregation degree
The effect mutually cooperateed with, stability and purifying water effect are superior, can be widely used in all kinds of waste water, industrial water and drinking water
Coagulating kinetics.This method has preparation process simple, and abundant raw material is cheap, and product stability is good, and floccule body forming is rapid,
The advantages that settling velocity is fast, and flocculating effect is good is suitable for promoting the use of.
Specific embodiment
The present invention provides a kind of methods for preparing flocculant with flyash and vanadium titano-magnetite, comprising the following steps:
A, vanadium titano-magnetite is crushed, it is spare；
B, the vanadium titano-magnetite for taking step a to obtain, is dissolved in NaOH solution, reacts 60~90min, takes supernatant liquor A；
C, flyash is taken, the HCl and H of 1~3 ︰ 1 of volume ratio is added2SO4, NaCl is added, it is permanent at a temperature of 25~35 DEG C
Warm 0.5~2.5h of magnetic agitation, obtains the mixture of fly ash of sour processing, takes supernatant liquor B；
D, by A liquid and B liquid, 1~5 ︰ 1 is mixed by volume, then the evaporative crystallization at 80~150 DEG C, obtains polysilicate wadding
Solidifying agent.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, magnetic iron ore described in step a is
The low-grade vanadium titano-magnetite of TFe content≤25%.Waste resource can be comprehensively utilized, the preparation cost of flocculant is saved.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, smashed granularity described in step a
To cross 160~200 meshes.The thinner the granularity of flyash and vanadium titano-magnetite the better, and slightly will lead to the reaction time excessively can be longer, instead
It should be not enough；The present invention select granularity for 160~200 meshes, be comprehensively consider crush cost and reaction effect after obtain
Optimal granularity.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, low grade vanadium titanium magnetic described in step b
The w/v of iron ore and NaOH are as follows: 3~6 ︰ 30~50.
Further, it is to go out to separate the gold in vanadium titano-magnetite using alkali soluble that the present invention, which adds the main purpose of NaOH solution,
Belong to salt ion.NaOH solution concentration is relatively low, is unfavorable for the dissolution of ionizable metal salt, higher, has unfavorable side reaction to generate, because
This, NaOH solution concentration of the present invention is 25~40%.The concentration of sodium hydroxide then flocculant yield less than normal is small, it is bigger than normal then
The flocculating effect of flocculant is bad.
In addition, the reaction time of vanadium titano-magnetite and NaOH are also very crucial, the reaction time, partially short then flocculant yield was reduced,
The reaction time flocculating effect of partially long then flocculant is impacted.The good flocculant of effect in order to obtain, vanadium titano-magnetite of the present invention
Reaction time with NaOH is 60~90min.
Further, in order to improve the yield and flocculating effect of flocculant, 1~3 ︰ 1 of volume ratio is added in step c of the present invention
HCl and H2SO4Carry out acidification reaction.The acidification reaction time is unsuitable too long, and the flocculating effect that otherwise will lead to flocculant is deteriorated.
Wherein, above-mentioned to be prepared in the method for flocculant with flyash and vanadium titano-magnetite, the additional amount of NaCl described in step c
Are as follows: NaCl1~4g is added in every 40~60g flyash.NaCl primarily serves dissolution assistant effect, and then its solubilization-aid effect on the low side is added in NaCl
It is not significant, it is on the high side to be unfavorable for H instead2SiO3Generation.
Present invention polysilicate flocculant produced, is a kind of water process high polymer coagulant, is with coal-burning power plant
Waste coal ash and the distinctive low-grade vanadium titano-magnetite of Panxi Diqu generate product through mixing, dipping, polymerization, evaporation, should
The metallic element that product contains also contains a small amount of vanadium and titanium, is that polysilicon acid is formed with Determination of multiple metal elements other than aluminium, calcium
Compound.The flocculant combines the advantages of iron AlSnSi alloy, weakens mutual weakness, not only have adsorption bridging effect with
Charge neutrality effect, have the function of molecule aggregation degree greatly, multicomponent mutually cooperate with, stability and purifying water effect are superior, can be wide
The general purified treatment applied to all kinds of waste water containing metal ion, industrial water and drinking water.
Present invention flyash and low-grade vanadium titano-magnetite produce polysilicate flocculant, using waste material as raw material, belong to
Regenerated resources exploitation, production cost is low, and added value of product is high, and the comprehensive utilization for flyash and low-grade v-ti magnetite provides
New approach has good economic benefit, environmental benefit and social benefit.
Present invention flyash and low-grade vanadium titano-magnetite produce polysilicate flocculant, and process is short, at low cost, investment
Few, product stability is good, and rapidly, settling velocity is fast, and decoloration performance is excellent, and the market competitiveness is strong for floccule body forming.
Explanation will be further explained to a specific embodiment of the invention by embodiment below, but do not indicated this
The protection scope of invention is limited in range described in embodiment.
Embodiment 1 prepares flocculant with the method for the present invention
It takes a certain amount of v-ti magnetite green ore to cross 200 mesh Tyler screens, it is stand-by to mix sampling.Weigh the stand-by v-ti magnetite of 4g
Green ore is dissolved in 30% 50mLNaOH solution, after reacting 90min, takes supernatant liquor A (hereinafter referred to as A liquid) stand-by.Claim
It takes 45g flyash in 500mL beaker, 1mol/LHCl and 1mol/LH is added2SO4Each 75mL adds 2g cosolvent NaCl,
The temperature constant magnetic stirring 1.0h at 28 DEG C, obtains the mixture of fly ash of sour processing, takes supernatant liquor B (hereinafter referred to as B liquid).By A:
B is uniformly mixed to arrive the glutinous thick liquid flocculant of light blue yellowish according to the ratio of volume ratio 3:1.In electric furnace function
Rate is evaporative crystallization under conditions of 150kw, obtains nattier blue chip solid flocculant.With the flocculant process copper-containing wastewater,
The removal rate of copper ion is up to 96%.
Embodiment 2 prepares flocculant with the method for the present invention
It takes a certain amount of v-ti magnetite green ore to cross 200 mesh Tyler screens, it is stand-by to mix sampling.Weigh the stand-by v-ti magnetite of 8g
Green ore is dissolved in 30% 100mLNaOH solution, after reacting 90min, takes supernatant liquor A (hereinafter referred to as A liquid) stand-by.Claim
It takes 90g flyash in 500mL beaker, 1mol/LHCl and 1mol/LH is added2SO4Each 150mL adds 4g cosolvent NaCl,
The temperature constant magnetic stirring 2.0h at 28 DEG C, obtains the mixture of fly ash of sour processing, takes supernatant liquor B (hereinafter referred to as B liquid).By A:
B is uniformly mixed to arrive the glutinous thick liquid flocculant of light blue yellowish according to the ratio of volume ratio 3:1.In electric furnace function
Rate is evaporative crystallization under conditions of 150kw, obtains nattier blue chip solid flocculant.With the flocculant process chromate waste water,
The removal rate of chromium ion is up to 90%.
Embodiment 3 prepares flocculant with the method for the present invention
It takes a certain amount of vanadium titano-magnetite and flyash to cross 200 mesh Tyler screens, it is stand-by to mix sampling.Weigh the stand-by vanadium of 2kg
Titanomagnetite raw ore is dissolved in 30% 25LNaOH solution, after reacting 90min, take supernatant liquor A (hereinafter referred to as A liquid) to
With.Flyash 3kg is weighed, 1mol/LHCl and 1mol/LH is added2SO4Each 50L adds 1.3kg cosolvent NaCl, at 28 DEG C
Lower temperature constant magnetic stirring 2.0h, obtains the mixture of fly ash of sour processing, takes supernatant liquor B (hereinafter referred to as B liquid).By A:B according to
The ratio of volume ratio 3:1 is uniformly mixed, and obtains the glutinous thick liquid flocculant of light blue yellowish.Evaporative crystallization obtains light
The chip solid flocculant of blue.With the waste water of the flocculant process chromate waste water and cupric, the removal of chromium ion and copper ion
Rate is 90% or more.
Claims (6)
1. the method for preparing flocculant with flyash and vanadium titano-magnetite, which comprises the following steps:
A, vanadium titano-magnetite is crushed, it is spare；
B, the vanadium titano-magnetite for taking step a to obtain, is dissolved in NaOH solution, reacts 60~90min, takes supernatant liquor A；
C, flyash is taken, HCl and H that volume ratio is 1~3 ︰ 1 is added2SO4, NaCl is added, the constant temperature magnetic force at 25~35 DEG C
0.5~2.5h is stirred, the mixture of fly ash of sour processing is obtained, takes supernatant liquor B；
D, by A liquid and B liquid, 1~5 ︰ 1 is mixed by volume, then the evaporative crystallization at 80~150 DEG C, obtains polysilicate flocculation
Agent.
2. the method according to claim 1 for preparing flocculant with flyash and vanadium titano-magnetite, it is characterised in that: step
Magnetic iron ore described in a is the low-grade vanadium titano-magnetite of TFe content≤25%.
3. the method according to claim 1 for preparing flocculant with flyash and vanadium titano-magnetite, it is characterised in that: step
Smashed granularity described in a was 160~200 meshes.
4. the method according to claim 1 for preparing flocculant with flyash and vanadium titano-magnetite, it is characterised in that: step
The weight ratio of low-grade vanadium titano-magnetite and NaOH described in b are as follows: 3~6 ︰ 30~50.
5. the method according to claim 1 for preparing flocculant with flyash and vanadium titano-magnetite, it is characterised in that: described
NaOH solution concentration be 25~40%.
6. the method according to claim 1 for preparing flocculant with flyash and vanadium titano-magnetite, it is characterised in that: step
The additional amount of cosolvent NaCl described in c are as follows: NaCl1~4g is added in every 40~60g flyash.
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Cited By (2)
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| CN113072151A (en) * | 2021-04-23 | 2021-07-06 | 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 |
| CN113072150A (en) * | 2021-04-22 | 2021-07-06 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary inorganic polymeric flocculant based on sulfuric acid acidolysis vanadium-titanium magnetite two-step method |
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| CN113072150A (en) * | 2021-04-22 | 2021-07-06 | 重庆理工大学 | Method for preparing iron-titanium-vanadium ternary inorganic polymeric flocculant based on sulfuric acid acidolysis vanadium-titanium magnetite two-step method |
| CN113072151A (en) * | 2021-04-23 | 2021-07-06 | 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 |
| 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 |
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