CN1683243A - Method and device for preparing synthetic zeolite from flyash zero discharged waste alkali liquid - Google Patents
Method and device for preparing synthetic zeolite from flyash zero discharged waste alkali liquid Download PDFInfo
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- CN1683243A CN1683243A CN 200510024185 CN200510024185A CN1683243A CN 1683243 A CN1683243 A CN 1683243A CN 200510024185 CN200510024185 CN 200510024185 CN 200510024185 A CN200510024185 A CN 200510024185A CN 1683243 A CN1683243 A CN 1683243A
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Abstract
The present invention relates to preparation process and apparatus of synthetic zeolite with flyash as material and no waste alkali liquid exhaust. Except traditional zeolite synthesizing reaction tank and solid-liquid separating dewatering tank, the apparatus has one additional dissolving tank for the component and alkalinity regulation and circulating use of waste alkali liquid. The preparation process includes reaction between flyash and sodium carbonate in the reaction tank to convert into zeolite, solid-liquid separating in the solid-liquid separating dewatering tank to obtain solid phase zeolite product and waste alkali liquid, regulating the Si/Al ratio of waste alkali liquid in the dissolving tank and returning the used alkali liquid into the reaction tank for reuse. The present invention has saving of alkali and water and eliminates environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method and device of flyash synthetic zeolite, the waste lye that produces in the Hydrothermal Preparation zeolite group mineral is carried out cycling and reutilization, realize the waste lye zero release in the zeolite production process.Belong to environmental protection technical field.
Background technology
Coal is important primary energy source, and its combustion processes also produces a large amount of by product-flyash except that obtaining energy.The flyash generation accounts for the 20-30% of coal weight, is one of maximum inoganic solids waste of global generation.The flyash year generation of major country is as follows: 6,000 ten thousand tons/year in the U.S.; 3,850 ten thousand tons/year in Europe; 100,000,000 6,000 ten thousand tons/year in China.Because flyash has certain coherency, part flyash is reused in the production of material of construction (cement, concrete etc.) at present.Its again utilization ratio be: U.S. 25-30%; Europe 48%; China about 40%.The most of flyash of all the other of Li Yonging is not stacked or landfill disposal by the original place, and the approach that utilizes again of therefore seeking new flyash has become the task of top priority.
Under this background, having occurred both at home and abroad with flyash in recent years is raw material synthetic zeolite mineral, thereby realizes the new trend of flyash high additive valueization.Because flyash is the product that inorganic components occurs behind high-temp combustion in the coal, original crystalline structure is destroyed mostly, except that a small amount of quartz and mullite, mainly based on the amorphous composition.Suitably improving under the alkaline condition of temperature, the composition in the flyash can produce reorganization, can produce zeolite group mineral thus.In recent years the low cost production high-level efficiency zeolite group mineral and expand and to have obtained many progress aspect the researchs such as application approach of zeolite product how, wherein the simplest suitable, with low cost, zeolite transformation efficiency height and most widely used synthetic method are hydrothermal synthesis methods.Application number is that 200410084313.6 Chinese invention patent " preparation method of flyash synthetic zeolite and application thereof " has proposed a kind of method of additive preparation high yield flyash synthetic zeolite and method that powder application coal ash synthetic zeolite is removed nitrogen phosphorus in the sewage synchronously of adding, adopt lower running cost and investment cost, solve the environmental problem that nitrogen phosphorus nutrition pollutent causes in flyash solid waste and the sewage, realize the resource utilization of nitrogen phosphorus in the resource utilization of flyash and the sewage simultaneously.
Yet, realize that by flyash be the extensive industrialization that raw material adopts hydrothermal method to prepare zeolite group mineral, the recontaminate problem of waste lye needs to be resolved hurrily.In Hydrothermal Preparation zeolite process, need to use a large amount of alkali lye, the general liquid-solid ratio that adopts is 3-10, that is to say that 1 ton of zeolite of every production will produce 3-10 ton waste lye.Concentration of lye generally reaches 1-5M (volumetric molar concentration).At this problem, need exploitation that waste lye is used in the technology that zeolite is produced, the pollution problem that had both solved waste lye, the usage quantity of saving alkali in the zeolite production process again again as alkali source, thereby the saving cost, and utilize the new approach of opening up again for the other industry waste lye.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of preparation method and device of flyash synthetic zeolite of waste lye zero release are proposed, with the less investment expense, both solved the environmental problem that the waste lye discharging causes, can save the cost of the required alkali of production process again, realize the resource utilization of flyash.
For realizing such purpose, it is raw material that the present invention adopts the flyash behind the coal burning, adds metal base solution and prepares zeolite group mineral by hydrothermal synthesis reaction, and solid phase is the synthetic zeolite product after solid-liquid separation; Liquid phase is waste lye.In the waste lye that produces, add and contain aluminium, siliceous grade can be in basic solution dissolved substances, adjust basicity, be back to the production of zeolite as alkali source.
The concrete grammar that the present invention prepares synthetic zeolite is:
1, residual solid waste coal ash is made raw material behind the employing coal burning, drop into zeolite compound reaction tank, add the metal base solution of 1～5M (volumetric molar concentration) in the ratio of liquid-solid ratio 3～20, thorough mixing, make into muddy, under 80～200 ℃ condition, reacted 3～48 hours, and finished by the conversion of flyash to zeolite.
2, reaction product is sent into dewatering tank, realize solid-liquid separation at this.Obtain the synthetic zeolite product after the solid phase cleaning, drying.Produce waste lye simultaneously.
3, waste lye is sent into dissolving tank through volume pump, add water and replenish alkali source, it is identical with former alkaline solution that its volume and basicity are adjusted to, and add can dissolved silicon or aluminum material waste lye is carried out the adjustment of Si/Al ratio, making the Si/Al ratio is 1.5～4, fully gets adjusted waste lye behind the stirring and evenly mixing.
According to the difference of flyash kind, the composition of waste lye is different.But common characteristic is other compositions such as iron content, calcium, magnesium, titanium not substantially, and different is or siliceous, or contains aluminium, and content also the kind because of flyash is different.Yet silicon and aluminium all are the main composition composition of zeolite lattice just.According to the kind of required synthetic zeolite, adding in waste lye can dissolved silicon or aluminum material.Once more, because the zeolite synthesis process need consumes alkali, the basicity of general waste lye is than the low 10-30% of former alkali lye.Therefore, except that regulating silica alumina ratio, also to replenish alkali source, make basicity reach the level of former alkali lye.
4, adjusted waste lye is sent into zeolite compound reaction tank, add flyash, begin the production of zeolite once more in the ratio of liquid-solid ratio 3～20, so move in circles, zeolite is constantly synthetic, do not discharge outside factory but do not produce waste lye, thus the zeolite production process of realization waste lye zero release.
The present invention is to realize the zero release of waste lye by the principal character of fly-ash Preparation synthetic zeolite, and realization preparation method's employing of the present invention is the new device of a cover, this device is characterised in that the combination that comprises following equipment: zeolite compound reaction tank, solid liquid separation dehydration tank, dissolving tank.In the device in traditional method existing zeolite compound reaction tank and the solid liquid separation dehydration tank, only need put a dissolving tank in addition, dissolving tank inside is provided with whipping appts, the import of dissolving tank links to each other with the waste lye outlet of solid liquid separation dehydration tank by flexible pipe, the outlet of dissolving tank links to each other with the inlet of zeolite compound reaction tank by flexible pipe, and volume pump is set respectively on the connecting pipeline of dissolving tank and zeolite compound reaction tank and solid liquid separation dehydration tank.Flyash and soda ash liquid realize that in zeolite compound reaction tank zeolite transforms, and converted product is realized solid-liquid separation in dewatering tank, when obtaining zeolite product, produce a large amount of waste lyes; Waste lye is not to be discharged in the environment, but is pumped into dissolving tank with metering.Dissolving tank is the device that is used for waste lye is carried out composition and basicity adjustment, so that waste lye meets or exceeds the level of soda ash liquid, realizes the waste lye recycling.
Compared with prior art, advantage of the present invention is conspicuous.Be to realize the utilization again of waste lye, only need to increase a dissolving tank with corresponding measuring pump and be connected flexible pipe on the basis of existing equipment, need not to do other transformation, running cost and investment cost are very low.Owing to there is not the discharging of waste lye in the production process, both saved the alkali cost, saved water resources again, and eliminated waste lye environment damage.Suitable adjusting by to the silica alumina ratio of waste lye can effectively utilize soluble silicon or aluminium in the waste lye, thereby improves the quality of zeolite product.Utilize the present invention can realize the resource utilization of solid waste (flyash), make full use of a large amount of fly ash of China and prepare synthetic zeolite, become a kind of environmental friendly material, can realize high additive valueization.Device of the present invention and zeolite preparation method can be applicable to the newly-built of hydrothermal method zeolite synthesis workshop or reconstruction, have both protected environment, save resource again, thereby are a kind of up-and-coming new technologies.
Description of drawings
Fig. 1 is raw material production synthetic zeolite and the apparatus structure synoptic diagram that reaches Zero discharge with flyash for the present invention.
Among Fig. 1,1 is the powdered coal ash measuring apparatus, and 2 is whipping appts, and 3 is zeolite compound reaction tank, and 4 is well heater, and 5 is dissolving tank, and 6 is volume pump, and 7 is flexible pipe, and 8 is solid liquid separation dehydration tank, and 9 is rinse bath, and 10 is drying installation, and 11 is finished product pack place.
Embodiment
Below in conjunction with drawings and Examples technical scheme of the present invention is further described.
The preparation facilities structure that embodiment adopts as shown in Figure 1, mainly comprise zeolite compound reaction tank 3, solid liquid separation dehydration tank 8 and dissolving tank 5, dissolving tank 5 link to each other with zeolite compound reaction tank 3 and solid liquid separation dehydration tank 8 by flexible pipe 7 respectively, and respectively volume pump 6 are set on connecting pipeline.The top inlet of zeolite compound reaction tank 3 is provided with powdered coal ash measuring apparatus 1, zeolite compound reaction tank 3 inside are provided with whipping appts 2, the bottom of zeolite compound reaction tank 3 is provided with well heater 4, the outlet of zeolite compound reaction tank 3 connects solid liquid separation dehydration tank 8 by a volume pump 6, the solid phase zeolite product outlet of solid liquid separation dehydration tank 8 is communicated with rinse bath 9 successively, drying installation 10, finished product pack place 11, the waste lye outlet of solid liquid separation dehydration tank 8 is connected to the import of dissolving tank 5 through volume pump 6 by flexible pipe 7.Dissolving tank 5 inside also are provided with whipping appts, and lower part outlet is connected to the top inlet of zeolite compound reaction tank 3 through volume pump by flexible pipe.
Flyash and soda ash liquid realize that in zeolite compound reaction tank 3 zeolite transforms, and converted product is realized solid-liquid separation in solid liquid separation dehydration tank 8, when obtaining the solid phase zeolite product, produce a large amount of waste lyes.Waste lye is sent into dissolving tank 5.Dissolving tank 5 is the devices that are used for waste lye is carried out composition and basicity adjustment, so that waste lye meets or exceeds the level of soda ash liquid, realizes the waste lye recycling.
Embodiment 1:
Residual solid waste coal ash is made raw material after adopting coal burning, after 1 weighing of powdered coal ash measuring apparatus, inserts in the zeolite compound reaction tank 3.In dissolving tank 5, modulate 1M (volumetric molar concentration) NaOH solution, be that 6 ratio is pumped into zeolite compound reaction tank with metering in liquid-solid ratio, both are used whipping appts 2 thorough mixing, make the zeolite compound reaction tank content remain on 95 ℃ of temperature with heating unit 4, and reacted with this understanding 24 hours, reaction product is pumped into solid-liquid separation with dewatering tank 8 with metering, makes solid phase and liquid phase separation at this.Solid phase is cleaned in rinse bath 9, drying installation 10 dryings, obtains zeolite product.Carry out packing in finished product pack place 11, dispatch from the factory then.The waste lye basicity that solid-liquid separation produces is 0.7M, waste lye is all sent in the dissolving tank 5 by volume pump 6 with flexible pipe 7.The volume of waste lye is 90% of a former alkali lye, makes volume identical with former alkali lye so add entry earlier.Regulate basicity to 1M (volumetric molar concentration) with solid NaOH, adding moisture water glass powder adjusting Si/Al ratio is 4, fully stirring and evenly mixing.Then waste lye is sent into zeolite compound reaction tank 3.Ratio in liquid-solid ratio 6 drops into flyash of the same race, reacted 24 hours down for 95 ℃ in temperature, and again with the solid phase drying after the solid-liquid separation, the zeolite product of getting back.Press cation exchange capacity and estimate the quality of zeolite product, the cation exchange capacity of this zeolite product is than previous round soda ash liquid synthetic zeolite product taller 30%.The raising of quality product is owing to soluble aluminum in the waste lye has obtained effective utilization in new round building-up process.
Residual solid waste coal ash is made raw material after adopting coal burning, after 1 weighing of powdered coal ash measuring apparatus, inserts in the zeolite compound reaction tank 3.In dissolving tank 5, modulate 2.5M (volumetric molar concentration) NaOH solution, be that 4 ratio is pumped into zeolite compound reaction tank 3 with metering in liquid-solid ratio, both are used whipping appts 2 thorough mixing, make the zeolite compound reaction tank content remain on 120 ℃ of temperature with heating unit 4, and reacted with this understanding 8 hours, reaction product is pumped into solid-liquid separation with dewatering tank 8 with metering, makes solid phase and liquid phase separation at this.Solid phase is cleaned in rinse bath 9, drying installation 10 dryings, obtains zeolite product, carries out packing in finished product pack place 11, dispatches from the factory then.The waste lye basicity that solid-liquid separation produces is 2.1M.By volume pump 6 waste lye is all sent in the dissolving tank 5.The volume of waste lye is 80% of a former alkali lye, makes volume identical with former alkali lye so add entry earlier.Regulate basicity to 2.5M (volumetric molar concentration) with solid NaOH, adding aluminium-hydroxide powder adjusting Si/Al ratio is 2, fully stirring and evenly mixing.Then waste lye is sent into zeolite compound reaction tank 3, dropped into flyash of the same race in the ratio of liquid-solid ratio 4, reaction is 8 hours under the condition of 120 ℃ of temperature, again with the solid phase cleaning, drying after the solid-liquid separation, the zeolite product of getting back.Press cation exchange capacity and estimate the quality of zeolite product, the cation exchange capacity of this zeolite product is than previous round soda ash liquid synthetic zeolite product taller 10%.The raising of quality product is owing to soluble silicon in the waste lye has obtained effective utilization in new round building-up process.
Residual solid waste coal ash is made raw material after adopting coal burning, after 1 weighing of powdered coal ash measuring apparatus, inserts in the zeolite compound reaction tank 3.In dissolving tank 5, modulate 2.0M (volumetric molar concentration) NaOH solution, be that 8 ratio is pumped into zeolite compound reaction tank with metering in liquid-solid ratio, both are used whipping appts 2 thorough mixing, make the zeolite compound reaction tank content remain on 95 ℃ of temperature with heating unit 4, and reacted with this understanding 6 hours, reaction product is pumped into solid-liquid separation with dewatering tank 8 with metering, makes solid phase and liquid phase separation at this.Solid phase is cleaned in rinse bath 9, drying installation 10 dryings, obtains zeolite product, carries out packing, dispatches from the factory in finished product pack place 11 then.The waste lye basicity that solid-liquid separation produces is 1.7M.By volume pump 6 waste lye is all sent in the dissolving tank 5.The volume of waste lye is 90% of a former alkali lye, makes volume identical with former alkali lye so add entry earlier.Regulate basicity to 2.0M (volumetric molar concentration) with solid NaOH, adding water glass powder adjusting Si/Al ratio is 1.8, fully stirring and evenly mixing.Then waste lye is sent into zeolite compound reaction tank 3, dropped into flyash of the same race in the ratio of liquid-solid ratio 8, reaction is 6 hours under the condition of 95 ℃ of temperature, again with the solid phase cleaning, drying after the solid-liquid separation, the zeolite product of getting back.6 times so repeatedly.Press cation exchange capacity and estimate the quality of zeolite product, use the cation exchange capacity ratio soda ash liquid synthetic zeolite product taller 15% of the zeolite product of the 5th waste lye production.The raising of quality product is owing to soluble aluminum in the waste lye has obtained effective utilization in building-up process.
Claims (2)
1, a kind of preparation method of flyash synthetic zeolite of waste lye zero release is characterized in that comprising the steps:
1) residual solid waste coal ash is made raw material behind the employing coal burning, drop into zeolite compound reaction tank (3), adding volumetric molar concentration in the ratio of liquid-solid ratio 3～20 is the metal base solution of 1～5M, and thorough mixing becomes muddy, reacts under 80～200 ℃ condition 3～48 hours;
2) reaction product of step 1 is sent into solid liquid separation dehydration tank (8) and carried out solid-liquid separation, solid phase is cleaned, obtain the synthetic zeolite product after the drying, produces waste lye simultaneously;
3) waste lye is sent into dissolving tank (5) through volume pump (6), add water and replenish alkali source, it is identical with former alkaline solution that its volume and basicity are adjusted to, and add can dissolved silicon or aluminum material waste lye is carried out the adjustment of Si/Al ratio, making the Si/Al ratio is 1.5～4, fully gets adjusted waste lye behind the stirring and evenly mixing;
4) adjusted waste lye is sent into zeolite compound reaction tank (3), added flyash, begin the production of zeolite once more, so move in circles, realize the zeolite production process of waste lye zero release in the ratio of liquid-solid ratio 3～20.
2, a kind of preparation facilities of flyash synthetic zeolite of waste lye zero release, comprise zeolite compound reaction tank (3), solid liquid separation dehydration tank (8), it is characterized in that also comprising dissolving tank (5), dissolving tank (5) inside is provided with whipping appts, the waste lye outlet of solid liquid separation dehydration tank (8) is connected to the import of dissolving tank (5) by flexible pipe (7), the lower part outlet of dissolving tank (5) is provided with volume pump (6) by hose connection top inlet to zeolite compound reaction tank (3) respectively on the connecting pipeline of dissolving tank (5) and zeolite compound reaction tank (3) and solid liquid separation dehydration tank (8).
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491363A (en) * | 2011-11-28 | 2012-06-13 | 中国环境科学研究院 | Device and method for synthesizing zeolite molecular sieves by solid waste materials |
| CN103408032A (en) * | 2013-07-21 | 2013-11-27 | 太原理工大学 | Method for supercritical hydrothermal synthesis of flyash zeolite |
| CN103738977A (en) * | 2013-12-27 | 2014-04-23 | 中国神华能源股份有限公司 | Method for preparing 4A type molecular sieve by taking white mud as raw material and product prepared by same |
| CN103949207A (en) * | 2014-05-05 | 2014-07-30 | 合肥工业大学 | Coal ash synthetic zeolite based nitrogen and phosphorus removing material as well as preparation and regeneration method thereof |
| CN116493378A (en) * | 2023-05-06 | 2023-07-28 | 中国华能集团清洁能源技术研究院有限公司 | System and method for comprehensively utilizing solid waste and treating wastewater of thermal power plant |
-
2005
- 2005-03-03 CN CN 200510024185 patent/CN1683243A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491363A (en) * | 2011-11-28 | 2012-06-13 | 中国环境科学研究院 | Device and method for synthesizing zeolite molecular sieves by solid waste materials |
| CN103408032A (en) * | 2013-07-21 | 2013-11-27 | 太原理工大学 | Method for supercritical hydrothermal synthesis of flyash zeolite |
| CN103408032B (en) * | 2013-07-21 | 2015-05-06 | 太原理工大学 | Method for supercritical hydrothermal synthesis of flyash zeolite |
| CN103738977A (en) * | 2013-12-27 | 2014-04-23 | 中国神华能源股份有限公司 | Method for preparing 4A type molecular sieve by taking white mud as raw material and product prepared by same |
| CN103738977B (en) * | 2013-12-27 | 2016-03-23 | 中国神华能源股份有限公司 | A kind of take white clay as the method that 4A type molecular sieve prepared by raw material and the product prepared by the method |
| CN103949207A (en) * | 2014-05-05 | 2014-07-30 | 合肥工业大学 | Coal ash synthetic zeolite based nitrogen and phosphorus removing material as well as preparation and regeneration method thereof |
| CN116493378A (en) * | 2023-05-06 | 2023-07-28 | 中国华能集团清洁能源技术研究院有限公司 | System and method for comprehensively utilizing solid waste and treating wastewater of thermal power plant |
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