CN1296129C - Method for synthesizing zeolite by fly ash and application thereof - Google Patents

Method for synthesizing zeolite by fly ash and application thereof Download PDF

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Publication number
CN1296129C
CN1296129C CNB2004100843136A CN200410084313A CN1296129C CN 1296129 C CN1296129 C CN 1296129C CN B2004100843136 A CNB2004100843136 A CN B2004100843136A CN 200410084313 A CN200410084313 A CN 200410084313A CN 1296129 C CN1296129 C CN 1296129C
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sewage
flyash
synthetic zeolite
fly ash
nitrogen
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CNB2004100843136A
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CN1631513A (en
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吴德意
孔海南
何圣兵
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上海交通大学
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Abstract

The present invention relates to a preparation method of fly ash synthetic zeolite and a method thereof applied to the field of synchronously removing the nitrogen and the phosphorus in sewage. Fly ash is used as a main raw material, is added with a substance which contains aluminium, silicon, chlorine or fluorine, etc., and can be dissolved in an alkaline solution. The fly ash and the substance are mixed and are added with a metal alkaline solution, and powder coal ash zeolite is synthesized through a hydrothermal synthesis reaction and then is transconformed and activated through a water-soluble metal salt solution. The fly ash synthetic zeolite is prepared after solid and liquid are separated. The transconformed and activated fly ash synthetic zeolite is prepared into granules and is filled in a filtration bed. The nitrogen and the phosphorus in sewage are synchronously removed through the synchronous adsorption cleaning capability of the fly ash synthetic zeolite for ammoniacal nitrogen and phosphate. Powdery fly ash synthetic zeolite can be directly put in the sewage to synchronously remove the nitrogen and the phosphorus. Simultaneously, the present invention solves the environmental problem caused by nitrogen and phosphorus nutrient pollutants in fly ash solid waste and the sewage to change the fly ash, and the nitrogen and the phosphorus in the sewage into resources, and the problem of secondary pollution can not be generated.

Description

The preparation method of flyash synthetic zeolite and application thereof

Technical field

The present invention relates to a kind of preparation method of flyash synthetic zeolite, and utilize the flyash synthetic zeolite to carry out the deep treatment method of sewage synchronous denitrification dephosphorizing, belong to environmental protection technical field.

Background technology

The seriously polluted key factor that influences the Chinese national economy sustainable development that become of shortage of water resources and water.Wherein eutrophication has become especially one of the most serious pollution of urban water-body of China's water body, must take measures to prevent and the comprehensive regulation, could improve water environment.At present, China's municipal sewage two stage treatment rate is improving constantly.But only depend on sewage second-level to handle and still can not remove the phosphorus and nitrogen that causes body eutrophication.In order to prevent and treat the body eutrophication environmental problem, need carry out the advanced treating of denitrogenation dephosphorizing to sewage, handle the solubility inorganic pollution material that the phosphorus, nitrogen etc. of being failed to remove can cause body eutrophication with further removal I and II.

Develop diversified deep treatment method at present, wherein had biological denitrificaion method, coagulant sedimentation, activated carbon filtration, ion-exchange, electrodialysis and film to handle or the like.But single usefulness wherein a kind of method generally can only be removed certain specific polluter from sewage; And carry out advanced treating by the treatment system of forming by several method, can increase investment cost again greatly, and cost such as operation and maintenance cost, and floor space is big, and the user is difficult to accept.Therefore very be necessary to develop nitrogen phosphorus in a kind of synchronous removal sewage, cost is low and operate easy technology.

Chinese patent CN1456520A discloses a kind of little flocculation-deep bed direct filtering and synchronously dephosphorizing and nitrogen removing new technology of municipal wastewater.The method of this process using is the combination of biological denitrificaion method and coagulant sedimentation, and promptly biological denitrificaion and coagulating sedimentation carry out in same filter tank, and the filter bed height surpasses to two times of common filter bed.Its advantage is a small investment, and floor space is little, is the activity of microorganism but the biological denitrificaion method relies on, and its treatment effect is subjected to easily such as temperature, the influence of environmental condition such as harmful substance in the sewage.

Ion-exchange also is one of denitrification treatment technology of normal employing at present, the ammonia nitrogen waste water of low concentration during this method is particularly suitable for.This technology not only cost is lower, and floor space is little, and the removal effect of ammonia nitrogen is not easy to be subjected to the influence of temperature.The ion-exchanger that generally uses is a natural zeolite at present.Obviously, when natural zeolite reaches capacity to the adsorption capacity of ammonia nitrogen, need re-use after its regeneration.And natural zeolite is to the adsorption capacity of ammonia nitrogen generally limited (for example China Zhejiang quality at home of producing the saturated adsorption capacity of Jinyun zeolite be 87cmol/kg) preferably, and that is to say needs be regenerated more continually, so just makes labour cost higher.In addition, zeolite is carried out frequent regeneration handle, the regeneration liquid measure that contains ammonia nitrogen in high density of generation is many, still needs further to its processing.On the other hand, natural zeolite can not be realized the purpose of dephosphorization simultaneously.

Summary of the invention

The objective of the invention is at the deficiencies in the prior art, a kind of preparation method of flyash synthetic zeolite and the method that powder application coal ash synthetic zeolite is removed nitrogen phosphorus in the sewage are synchronously proposed, adopt lower operating cost and investment cost, solve the environmental problem that nitrogen phosphorus nutrition pollutant causes in flyash solid discarded object and the sewage, realize the resource of nitrogen phosphorus in the resource of flyash and the sewage simultaneously.

For realizing such purpose, it is primary raw material that the present invention adopts the flyash behind the coal burning, add and contain aluminium, siliceous, chloride or fluorine-containing etc. can be in alkaline solution dissolved substances, mixing the back adds metal base solution and by the synthetic coal ash zeolite of hydrothermal synthesis reaction, through activation transition of water miscible metal salt solution, makes the flyash synthetic zeolite after Separation of Solid and Liquid again.Flyash synthetic zeolite after activation transition is made particle packing in filter bed, utilize the flyash synthetic zeolite, realize the synchronous denitrification dephosphorizing of sewage is handled ammonia nitrogen and phosphatic synchronous adsorption cleaning ability.Also Powdered flyash synthetic zeolite directly can be added in sewage treatment plant's second pond sewage or in other nitrogenous phosphorus sewage, realize synchronous denitrification dephosphorizing.

The concrete grammar that the present invention prepares the flyash synthetic zeolite is:

1, residual solid waste coal ash is made raw material behind the employing coal burning, interpolation can be dissolved in alkaline solution contains aluminium, siliceous, chloride or fluorine-containing material is prepared burden, and wherein aluminium-containing substance is 0～50% of a flyash weight, and silicon-containing material is 0～30% of a flyash weight, chlorine-bearing compound is 0～50% of a flyash weight, fluorine-containing material is 0～50% of a flyash weight, and the batching of interpolation can be one or more, and total addition level is at 20-60%.

2, get the metal base solution that molar concentration is 1～5M, mix in the ratio of liquid-solid ratio 1.5～20 with the flyash after adding batching, reacted 3～48 hours in the airtight or open system under 80～200 ℃,, and will obtain coal ash zeolite after the solid phase drying through Separation of Solid and Liquid.

3, to the coal ash zeolite activation that makes the transition, adopt water-soluble, harmless to biology, (molar concentration of metal ion is 0.1～5M) to the metal salt solution more than the divalence, with the ratio mixing of coal ash zeolite in liquid-solid ratio 1.5～20, Separation of Solid and Liquid again after saturated processing, the salts substances that flush away does not adsorb, drying, the flyash synthetic zeolite after obtaining activating.

The flyash synthetic zeolite principal character of the present invention's preparation is an energy denitrogenation dephosphorizing simultaneously, and detergent power is strong, and the nitrogen phosphorus that can be applied to sewage purifies advanced treating.

Flyash synthetic zeolite after activation transition is made 2～20mm particle, behind air dry or the heat drying, fill in the Filter column, be used for removing the nitrogen phosphorus in the sewage.Sewage is sent into the Filter column from the Filter column bottom by measuring pump, and outlet of sewer is arranged at the Filter column upper end, is higher than filling surface 50～250mm, is lower than filter capital end 200～500mm.The height of Filter column is 0.8～3m, internal diameter 100～300mm, filter bed height 0.5～2.5m.The design of effluent flow rate so that the time of staying of sewage in filter bed be to be advisable in 2 minutes to 60 minutes.Sewage is in through the filter bed process of being filled by the flyash synthetic zeolite, and nitrogen wherein (ammonia nitrogen) and phosphorus polluters such as (phosphate) will be adsorbed fixing by the flyash synthetic zeolite, and sewage is purified.

The flyash synthetic zeolite generally is higher than maximum processing capability to nitrogen to the maximum processing capability of phosphorus.After the adsorption capacity to nitrogen phosphorus reached capacity, (molar concentration of metal ion was 0.1～5M) to carry out wash-out regeneration can to adopt the water-soluble metal salting liquid to the absorption crystallized ability of ammonia nitrogen.

If handle the sewage do not contain biological harmful pollutants (for example sanitary sewage etc.), also can not adopt the regeneration measure, the flyash synthetic zeolite filler that upgrades in the filter post can restart running.And the flyash synthetic zeolite that is adsorbed with nitrogen phosphorus can be used for the improvement of agricultural land soil.

The other method that the flyash synthetic zeolite is applied to the nitrogen phosphorus purification advanced treating of sewage is directly Powdered flyash synthetic zeolite to be added in sewage treatment plant's second pond sewage or in other nitrogenous phosphorus sewage, nitrogen phosphorus nutrition pollutional load is handled, and dosage is 0.5～8kg/ ton sewage.This method of operating is more simple, and need not any equipment or facility, can carry out in existing sewage treatment facility.Flyash synthetic zeolite after adsorption cleaning is finished enters second pond mud, handles together to get final product when second pond mud is cleared up.

Compared with prior art, the present invention has the following advantages:

(1) the denitrogenation dephosphorizing advanced treatment method for sewage water of the present invention's proposition is owing to finish by the materialization adsorption cleaning process of flyash synthetic zeolite, need not to add other materials, also not having special operating condition needs control, the shortcoming of having avoided the treatment effect of microbial method influenced by temperature etc.

(2) device fairly simple (Filter column method) even need not other adding set (directly adding method), operation is relatively easy, and does not take a large amount of land areas.Therefore operating cost and investment cost are low.

Therefore (3), use the flyash synthetic zeolite to substitute natural zeolite centering, NITROGEN IN LOW CONCENTRATION phosphorus waste water is handled, and can reduce the regeneration frequency because the flyash synthetic zeolite is big to the adsorption capacity of ammonia nitrogen.With synthetic saturated adsorption capacity is that the flyash synthetic zeolite of 220cmol/kg is an example, and its regeneration frequency is compared with the Jinyun county, Zhejiang province natural zeolite and can be reduced by 2.5 times, thereby saves the required labour of regenerative process greatly.

(4) another key character of the present invention is the pollution problem of nitrogen phosphorus in solving sewage, also can realize the resource of solid waste (flyash).Flyash is one of main solid waste of China, by the preparation coal ash zeolite and through activation transition, becomes a kind of environmental friendly material, can realize high additive valueization, thereby be a kind of up-and-coming new technology.

(5) so long as the nitrogen phosphorus waste water (for example sanitary sewage after the biochemical treatment) that does not contain hazardous substance is handled, the flyash synthetic zeolite that contains high concentration N-P after absorption reaches capacity can be applied in the farmland.The flyash synthetic zeolite itself has the effect of improvement agricultural land soil, especially promotes the formation of soil aggregate and the improvement of fertilizer-preserving ability.Be applied to the farmland again behind the treated nitrogenous phosphorus waste water, the nitrogen phosphorus of absorption can utilize for crops, thereby can save the fertilizer spending and alleviate the agricultural wastewater pollution problem.Therefore present technique can solve the environmental problem that nitrogen phosphorus nutrition pollutant causes in flyash solid discarded object and the sewage simultaneously, and can realize the resource of nitrogen phosphorus in the resource of flyash and the sewage simultaneously, also can not produce secondary pollution problem.

Description of drawings

Fig. 1 is the direct filter bed method processing nitrogen phosphorus waste water schematic diagram of filler with the flyash synthetic zeolite for the present invention.

Among Fig. 1,1 is delivery port, and 2 is flyash synthetic zeolite filtering layer, and 3 are pressure measurement and sample tap, and 4 is supporting layer, and 5 are the backwash water inlet, and 6 are the backwash air inlet, and 7 is measuring pump.

The specific embodiment

Below in conjunction with drawings and Examples technical scheme of the present invention is further described.

Embodiment 1:

Residual solid waste coal ash is made raw material after adopting coal burning, adds sodium metasilicate, and salt is prepared burden, and wherein sodium metasilicate is 20% of a flyash weight, and salt is 40% of flyash weight.Getting 1M (molar concentration) NaOH solution, is that 6 ratio is mixed with flyash after adding batching in liquid-solid ratio, reacts 24 hours down for 95 ℃ in temperature, again with the solid phase drying after the Separation of Solid and Liquid, obtains the flyash synthetic zeolite.Then the flyash synthetic zeolite is activated transition, adopt 0.5M CaCl 2Solution, with the ratio mixing of coal ash zeolite in liquid-solid ratio 5, Separation of Solid and Liquid again after saturated processing, the salts substances that flush away does not adsorb, drying change into the calcium type flyash synthetic zeolite that nitrogen phosphorus in the sewage is had adsorption activity.

To be pressed into the particle of 2～4mm through the flyash synthetic zeolite of activation transition, fill in after drying in the filter post, be used for removing the phosphorus and nitrogen in the sewage.As shown in Figure 1, be pre-charged with certain thickness gravel supporting layer 4 below 2 to help into water and backwash at flyash synthetic zeolite filtering layer.The thickness of supporting layer 4 is 80mm, and the thickness of flyash synthetic zeolite filtering layer 2 is 800mm, filter column internal diameter 150mm.The design of filtering velocity is to make that the time of staying of sewage in filtering layer is 20 minutes.The lower end of filter post is connected to sewage inlet port, backwash water inlet 5 and backwash air inlet 6.Delivery port 1 is positioned at the upper end of filter post, from flyash synthetic zeolite filtering layer 2 top 120mm.Filter material layer is provided with pressure measurement and sample tap 3 every 200mm.Sewage enters filler adsorbed purification that nitrogen phosphorus in the flow through process of flyash synthetic zeolite filtering layer 2 in sewage by flyash synthetic zeolite constituted by design current velocity from the filter column bottom by measuring pump 7.Untreated sewage contains ammonia nitrogen 40mg/L, phosphorous 3.5mg/L.Adsorption cleaning efficient is: ammonia nitrogen 52%, phosphorus 70%.

Embodiment 2

Add sodium metasilicate and sodium fluoride in flyash, sodium metasilicate is 5% of a flyash weight, and sodium fluoride is 20% of a flyash weight.Getting 2M (molar concentration) NaOH solution, is that 10 ratio is mixed with flyash after adding batching in liquid-solid ratio, reacts 24 hours down for 120 ℃ in temperature, again with the solid phase drying after the Separation of Solid and Liquid, obtains coal ash zeolite.Then the flyash synthetic zeolite is activated transition, adopt 0.5M (molar concentration) CaCl 2Solution, with the ratio mixing of coal ash zeolite in liquid-solid ratio 8, Separation of Solid and Liquid again after saturated processing repeatedly, the salts substances that flush away does not adsorb, drying change into the saturated flyash synthetic zeolite of calcium that nitrogen phosphorus in the sewage is had adsorption activity.

To be pressed into the particle of 8mm through the flyash synthetic zeolite of activation transition, fill in after drying in the filter post, be used for removing the phosphorus and nitrogen in the sewage.As shown in Figure 1, the thickness of supporting layer 4 is 80mm, and the thickness of flyash synthetic zeolite filtering layer 2 is 800mm, filter column internal diameter 150mm.The design of filtering velocity is to make that the time of staying of sewage in filtering layer is 30 minutes.The lower end of filter post is connected to sewage inlet port, backwash water inlet 5 and backwash air inlet 6.Delivery port 1 is positioned at the upper end of filter post, from flyash synthetic zeolite filtering layer 2 top 120mm.Filter material layer is provided with pressure measurement and sample tap 3 every 200mm.Sewage enters filter post, filler adsorbed purification that nitrogen phosphorus in the flow through process of flyash synthetic zeolite filtering layer 2 in sewage by flyash synthetic zeolite constituted by design current velocity from the filter column bottom by measuring pump 7.Untreated sewage contains ammonia nitrogen 30mg/L, phosphorous 4mg/L.Adsorption cleaning efficient is: ammonia nitrogen 45%, phosphorus 65%.

Embodiment 3

Add metal aluminum foil and sodium chloride in flyash, wherein aluminium foil is 5% of a flyash weight, and sodium chloride is 30% of flyash weight.Metal base solution is got 1M (molar concentration) NaOH solution, is that 5 ratio is mixed with flyash after adding batching in liquid-solid ratio, reacts 16 hours down for 95 ℃ in temperature, again with the solid phase drying after the Separation of Solid and Liquid, obtains coal ash zeolite.Then the flyash synthetic zeolite is activated transition, adopt 0.5M (molar concentration) FeCl 3Solution, with the ratio mixing of coal ash zeolite in liquid-solid ratio 8, Separation of Solid and Liquid again after saturated processing, the salts substances that flush away does not adsorb, drying change into the saturated flyash synthetic zeolite of calcium that nitrogen phosphorus in the sewage is had adsorption activity.

The flyash synthetic zeolite of activation directly adds in sewage through transition, and dosage is a 5kg/t sewage, 60 minutes times of contact.Sewage contains ammonia nitrogen 25mg/L, phosphorous 2mg/L before handling.Adsorption cleaning efficient is: ammonia nitrogen 55%, phosphorus 80%.

Claims (1)

1, a kind of flyash synthetic zeolite that utilizes carries out sewage synchronous denitrification dephosphorizing deep treatment method, it is characterized in that comprising the steps:
1) adopts pulverized fuel ash as raw materials, interpolation can be dissolved in alkaline solution contains aluminium, siliceous, chloride or fluorine-containing material is prepared burden, and wherein aluminium-containing substance is 0～50% of a flyash weight, and silicon-containing material is 0～30% of a flyash weight, chlorine-bearing compound is 0～50% of a flyash weight, fluorine-containing material is 0～50% of a flyash weight, and the batching of interpolation is above-mentioned one or more, and total addition level is at 20-60%;
2) get the metal base solution that molar concentration is 1～5M, mix in the ratio of liquid-solid ratio 1.5～20 with the flyash after adding batching, reacted 3～48 hours in the airtight or open system under 80～200 ℃,, and will obtain the flyash synthetic zeolite after the solid phase drying through Separation of Solid and Liquid;
3) adopting the metal ion molar concentration is the water-soluble metal salting liquid of 0.1～5M, with the ratio mixing of flyash synthetic zeolite in liquid-solid ratio 1.5～20, Separation of Solid and Liquid again after saturated processing, the salts substances that flush away does not adsorb, drying, the flyash synthetic zeolite after obtaining activating;
4) with the particle packing of flyash synthetic zeolite in Filter column, the height of Filter column is 0.8～3m, internal diameter 100～300mm, the thickness of flyash synthetic zeolite filtering layer (2) is 0.5～2.5m, filling thickness is the gravel supporting layer (4) of 80mm below flyash synthetic zeolite filtering layer (2), the lower end of filter post is connected to the sewage inlet port, backwash water inlet (5) and backwash air inlet (6), outlet of sewer is arranged on the Filter column upper end, be higher than filling surface 50～250mm, be lower than filter capital end 200～500mm, sewage is sent into the Filter column from the Filter column bottom by measuring pump, and the time of staying of sewage in filter bed is 2-60 minute; Perhaps, Powdered flyash synthetic zeolite is directly added in sewage, nitrogen phosphorus nutrition pollutional load is handled, dosage is 0.5～8kg/ ton sewage.
CNB2004100843136A 2004-11-18 2004-11-18 Method for synthesizing zeolite by fly ash and application thereof CN1296129C (en)

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