CN103664242A - Caustic sludge treatment method - Google Patents
Caustic sludge treatment method Download PDFInfo
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- CN103664242A CN103664242A CN201310430904.3A CN201310430904A CN103664242A CN 103664242 A CN103664242 A CN 103664242A CN 201310430904 A CN201310430904 A CN 201310430904A CN 103664242 A CN103664242 A CN 103664242A
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Abstract
The invention discloses a caustic sludge treatment method and belongs to the field of chemical industry environment treatment. The problem of environmental pollution caused by caustic sludge stacking is solved. The treatment method comprises the following steps: pretreating a potassium feldspar raw material, drying and roasting, leaching, evaporating to prepare low sodium salt, performing potassium chloride crystallization, performing calcium chloride granulation and treating the caustic sludge and alkali liquor. The potassium feldspar and salty mud are taken as raw materials, the caustic sludge generated in the process of producing sodium carbonate through an ammonia-soda process is treated, the problem of environmental pollution caused by caustic sludge stacking is solved, the domestic quantity demand of potash fertilizers is met, and the caustic sludge treatment method is low in raw material cost, simple in process and easy to operate.
Description
Technical field
The invention belongs to chemical environment and administer field, be specifically related to a kind for the treatment of process of alkaline residue.
Background technology
Alkaline residue is the waste residue producing in ammonia-soda process soda ash process, and production practice prove that one ton of soda ash of every production need discharge 0.3～0.5 ton of solid-state waste residue, a large amount of waste residues store up a large amount of soil that both accounted for, caused again serious environmental pollution.
Alkaline residue is stored up processing except building a dam at present, is mainly used in cement processed, engineering soil etc.As CN1140151A discloses the method for a kind of alkaline residue engineering purposes processed, the method for alkaline residue cement processed attempts alkaline residue to become useful product, but implement comparatively difficulty, cost is also high; The method of producing engineering soil from alkaline slag adopts stirring means to change alkaline residue structure; make it to be easy to dehydration; after conventional airing, be used as engineering earth; better performances; for mass-producing, administer alkaline residue and opened up road, but products obtained therefrom is only done engineering purposes, economic value added is lower; this method biases toward processing alkaline residue, the useful component in alkaline residue can not be fully utilized.
The potash fertilizer of China shortage at present, every year need be from a large amount of potash fertilizer of external import, China's soluble potassium ore resources reserves are few, China's large-scale development be only the higher bittern potassium resource of grade, as Qinghai Chaerhan salt lakes etc., along with the increase of potash fertilizer demand, the minimizing of soluble potassium ore resources, how to develop soluble potassium resource, become China's task of top priority.
Summary of the invention
In view of above-mentioned problems of the prior art, the present invention proposes a kind of method of utilizing alkaline residue to prepare potash fertilizer, both solve alkaline residue and stacked the problem of environmental pollution causing, also met the domestic demand to potash fertilizer.
Technical solution of the present invention comprises:
A treatment process for alkaline residue, this treatment process comprises the following steps:
1) take a certain amount of potassium felspar sand raw material and be crushed to 100～200 orders, then by source material delivery system, being sent in blender;
2) in above-mentioned blender, add alkaline residue, it is mixed with potassium felspar sand raw material, the weight ratio of described alkaline residue and potassium felspar sand is 0.5～3.0:1,
3) alkaline residue step 2) mixing and potassium felspar sand raw material are sent in Reaktionsofen and are carried out roasting, obtain gas and compound, and gas is through cascade filtration remanufacture dry ice, scrubbing dust collection qualified discharge;
4) compound in step 3) is sent in the leacher that leaching liquid is housed, and after heating, be incubated, stir, delivers in plate-and-frame filter press and carries out press filtration separation, obtains filtrate one and filter residue one;
5) filtrate in step 4) one is sent in vaporizer and evaporated, collect resultant sodium-chlor, Repone K and calcium chloride;
6) by sending into acidification pool after one washing of the filter residue in step 4), press filtration, through acidifying, make metal ion ionization wherein, then through in plate-and-frame filter press, carry out press filtration separation, obtain filtrate two and filter residue two;
7) will after two washings of the filter residue in step 6), press filtration, send in the molten reactor of alkali, after alkalinisation treatment, press filtration separation, obtain filtrate three and insoluble filter residue three, described filtrate three is water glass mother liquor, described water glass mother liquor is for the production of metasilicate pentahydrate sodium or white carbon black, and filter residue three is as cement clinker;
8) filtrate in step 6) two is delivered in acidification reaction still, through acidification, made the whole ionizations of metallic cation, obtain filtrate four and filter residue four after press filtration separation, filtrate four is carried out to acidification, press filtration separation obtains ironic hydroxide and filtrate five;
9) by step 8) in filtrate five carry out acidification, press filtration separation obtains aluminium hydroxide and ammonium sulfate.
Above-mentioned steps 2) in blender, add salt slurry, the weight ratio of described salt slurry and potassium felspar sand is 0.001～0.5:1.
Above-mentioned steps 3) in, Reaktionsofen is that suspension preheating burns stove, and maturing temperature is 800～1200 ℃, and roasting time is 30～90min.
Above-mentioned steps 4) leaching liquid in is evaporated waste ammonia liquid.
Above-mentioned steps 7) in, in the molten reactor of alkali, be sodium hydroxide solution, be strong basicity after sodium hydroxide alkalization is processed.
The useful technique effect that the present invention brings:
The present invention proposes a kind for the treatment of process of alkaline residue, it selects potassium felspar sand and salt slurry is that raw material is processed the alkaline residue producing in ammonia-soda process soda ash process, solve alkaline residue and stacked the problem of environmental pollution causing, treatment process of the present invention comprises: roasting, leaching, evaporation collection sodium-chlor, Repone K and calcium chloride, the operations such as separation, finally prepare soluble potassium salt, met the domestic demand to potash fertilizer; Raw materials cost of the present invention is low, technique simple, easy handling.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is done to further clear, complete explanation:
Fig. 1 is process flow sheet of the present invention.
Embodiment
Material handling of the present invention is the alkaline residue producing in ammonia-soda process soda ash process, selected raw material is mainly potassium felspar sand and salt slurry, potassium felspar sand molecular formula is: KAlSi3O8, the main component of salt slurry is Mg (OH) 2, CaC03, BaSO4, the selected raw material of the present invention, except special instruction, all can be bought and be obtained by commercial channel.
A treatment process for alkaline residue, this treatment process comprises the following steps:
Step 1: first potassium felspar sand raw material is sent into jaw crusher and pulverized, then to 100 order～200 orders, by transporting system for raw materials, deliver to blender through in small, broken bits, standby;
Step 2: respectively alkaline residue and salt slurry are sent in agitator and mixed by screw feeder by a certain percentage, send into again in moisture eliminator dry, moisture drying in compound is gone out, and dried material is sent into mixing tank, sneaks in proportion the potassium felspar sand raw material of step 1;
Step 3: after potassium felspar sand raw material mixes (calling compound in the following text) with dried alkaline residue, salt slurry in step 2, by screw feeder, send into suspension preheating and burn kiln roasting, stoving oven out gas, remove dried material in spray-dryer, dried gas is extracted out through cyclone dust removal, the gas producing absorbs remanufacture dry ice, scrubbing dust collection rear discharge up to standard after cascade filtration;
Step 4: the compound in step 3 is sent in the leacher that leaching liquid is housed, after heating, be incubated, stir, delivers in plate-and-frame filter press and carries out press filtration separation, obtains filtrate one and filter residue one;
Step 5: the filtrate in step 4 one is sent in vaporizer and evaporated, collect resultant sodium-chlor, Repone K and calcium chloride; These step concrete operations are:
A, evaporation Cardia Salt processed workshop section
The filtrate one of step 4 enters in vaporizer evaporates, filtrate one is introduced into the evaporation of multiple-effect evaporator multiple-effect program, the raw steam heating one effect vaporization cycle liquid that boiler comes, steam condensate is sent boiler back to through block steam and drain water device and water extraction pump and is recycled, the secondary steam that one effect evaporation produces is used for heating two effect circulation fluids, time condensation water is sent into the equipment such as each vaporizer and whizzer for cleaning through block steam and drain water and a water extraction pump, two effect evaporations produce steam and are used for heating triple effect circulation fluid, three times water of condensation is sent into the equipment such as each vaporizer and whizzer for cleaning through block steam and drain water and a water extraction pump, through surface condenser condensate vacuum pump, bleed and make triple effect keep certain negative pressure, water coolant adopts recirculated water.
Through the most of crystallization of evaporation post chlorization sodium, a small amount of crystallization of Repone K, the salt that contains Repone K and sodium-chlor slurry, after thickener, clear liquid flows into mother liquor tank, dense salt slurry is sent into whizzer centrifugation, and liquid phase enters mother vat, and the salt of chloride containing potassium is through processing Cardia Salt processed;
B, Repone K crystallization workshop section
After the mother liquor that evaporation comes and the mother liquor heat exchange after Repone K Crystallization Separation, cooling, deliver to crystallization, cooling and separate out Repone K due to vacuum action, the steam of being discharged by crystallizer enters surface condenser, and is vacuumized by vacuum pump, guarantees the vacuum tightness of crystallizer;
After two-stage crystallization, containing the dense salt slurries thickener of crystallization, clear liquid flows into potassium mother vat, and sylvite slurry is separated through whizzer, and mother liquor is sent into potassium mother vat, sylvite through rotary conveyor, fluidised bed drying, cooling, send to packing again and be finished product Repone K.Be dried and supplied with by gas blower with warm air, airheater heating, combustion gas is through cyclone dust removal.After scrubbing dust collection, discharge, washing recycles and does not discharge with waste clear solution;
Mother liquor of calcium is delivered to roasting workshop section by a pump part and is prepared burden, the potassium mother liquor heat exchange that a part is come through interchanger and evaporation.Dechlorination calcium pelleting workshop section after heat exchange;
C, calcium chloride granulation workshop section
Mother liquor from Repone K crystallization workshop section enters settling tank clarification, clear liquid flows into calcium liquid bath, magma is put into magma groove, by magma pump, return potassium crystallization thickener again, calcium liquid enters climbing-film evaporator through preheater preheating, climbing-film evaporation fluid is sprayed onto fluidized-bed layer by being pumped to fog system, dark liquid is sprayed by twin nipple with pressurized air, owing to adopting heated dry air, ambient air preheating in the heat exchanger of an internal cooling circulation, finally by combustion of natural gas, it is heated to 48 ℃ indirectly, dry tail gas is out through cyclone dust removal scrubbing dust collection qualified discharge.
Step 6: by sending into acidification pool by conveyor after one washing of the filter residue in step 4, press filtration, make metal ion ionization wherein through acidifying, then carry out press filtration separation through in plate-and-frame filter press, obtain filtrate two and filter residue two;
Step 7: will send in the molten reactor of alkali after two washings of the filter residue in step 6, press filtration, after alkalinisation treatment, press filtration separation, obtain filtrate three and insoluble filter residue three, described filtrate three is water glass mother liquor, described water glass mother liquor is for the production of metasilicate pentahydrate sodium or white carbon black, the main component of filter residue three is tricalcium silicate, Dicalcium Phosphate (Feed Grade), directly as cement clinker;
Step 8: the filtrate in step 6 two is delivered in acidification reaction still, through acidification, make the whole ionizations of metallic cation, after press filtration separation, obtain filtrate four and filter residue four, filtrate four is carried out to acidification, by regulating pH, press filtration separation to obtain ironic hydroxide and filtrate five;
Step 9: the filtrate in step 8 five is carried out to acidification, regulate pH, press filtration separation to obtain aluminium hydroxide and ammonium sulfate.
Below in conjunction with specific embodiment, the present invention is done to further clear, complete explanation:
Embodiment 1:
Step 1: potassium felspar sand, alkaline residue and salt slurry are mixed by the weight ratio of 1:1.5:0.2, be crushed to 100 orders in ball mill;
Step 2: the potassium felspar sand mixing, alkaline residue and salt slurry are put into suspension preheating and burn kiln roasting, at the temperature of 1200 ℃, sintering is 1 hour, be dissolved in water after taking-up sinter boiling 10 minutes, after centrifugation precipitation by concentrated Cardia Salt, Repone K, the calcium chloride of obtaining respectively of clear liquid;
Step 3: isolated residue separated liquid obtaining after acid treatment regulates pH, and making pH is 7～8, then carries out press filtration separation through in plate-and-frame filter press, makes respectively ironic hydroxide and aluminium hydroxide; Insoluble residue adds 20%-35% sodium hydroxide and is adjusted to strong basicity in reactor, boil dissolving, and maintain strong basicity all the time, the mixture centrifugation obtaining after half an hour, isolated precipitation centrifuge dehydration obtains cement clinker, the concentrated Starso that obtains of isolated clear liquid.
Embodiment 2:
Step 1: potassium felspar sand, alkaline residue and salt slurry are mixed by the weight ratio of 1:1:0.5, be crushed to 100 orders in ball mill;
Step 2: the potassium felspar sand mixing, alkaline residue and salt slurry are put into suspension preheating and burn kiln roasting, at the temperature of 1000 ℃, sintering is 1.5 hours, be dissolved in water after taking-up sinter boiling 30 minutes, after centrifugation precipitation by concentrated Cardia Salt, Repone K, the calcium chloride of obtaining respectively of clear liquid;
Step 3: isolated residue separated liquid obtaining after acid treatment makes respectively ironic hydroxide and aluminium hydroxide by tune pH; Insoluble residue hydro-oxidation sodium in reactor regulates pH to maintain strong basicity, boil dissolving, and remain strong basicity, the mixture centrifugation obtaining after half an hour, isolated precipitation centrifuge dehydration obtains cement clinker, the concentrated Starso that obtains of isolated clear liquid.
Should be understood that; the above-mentioned description for embodiment is comparatively detailed; can not therefore think the restriction to scope of patent protection of the present invention; those of ordinary skill in the art is under enlightenment of the present invention; do not departing from the scope situation that the claims in the present invention protect; can also make the various deformation such as replacement, simple combination, the scope of asking for protection of the present invention should be as the criterion with claims.
Claims (5)
1. a treatment process for alkaline residue, is characterized in that the treating method comprises following steps:
1) take a certain amount of potassium felspar sand raw material and be crushed to 100～200 orders, then by source material delivery system, being sent in blender;
2) in above-mentioned blender, add alkaline residue, it is mixed with potassium felspar sand raw material, the weight ratio of described alkaline residue and potassium felspar sand is 0.5～3.0:1,
3) alkaline residue step 2) mixing and potassium felspar sand raw material are sent in Reaktionsofen and are carried out roasting, obtain gas and compound, and gas is through cascade filtration remanufacture dry ice, scrubbing dust collection qualified discharge;
4) compound in step 3) is sent in the leacher that leaching liquid is housed, and after heating, be incubated, stir, delivers in plate-and-frame filter press and carries out press filtration separation, obtains filtrate one and filter residue one;
5) filtrate in step 4) one is sent in vaporizer and evaporated, collect resultant sodium-chlor, Repone K and calcium chloride;
6) by sending into acidification pool after one washing of the filter residue in step 4), press filtration, through acidifying, make metal ion ionization wherein, then through in plate-and-frame filter press, carry out press filtration separation, obtain filtrate two and filter residue two;
7) will after two washings of the filter residue in step 6), press filtration, send in the molten reactor of alkali, after alkalinisation treatment, press filtration separation, obtain filtrate three and insoluble filter residue three, described filtrate three is water glass mother liquor, described water glass mother liquor is for the production of metasilicate pentahydrate sodium or white carbon black, and filter residue three is as cement clinker;
8) filtrate in step 6) two is sent in acidification reaction still, through acidification, made the whole ionizations of metallic cation, obtain filtrate four and filter residue four after press filtration separation, filtrate four is carried out to acidification, press filtration separation obtains ironic hydroxide and filtrate five;
9) by step 8) in filtrate five carry out acidification, press filtration separation obtains aluminium hydroxide and ammonium sulfate.
2. treatment process according to claim 1, is characterized in that: described step 2) in blender, add salt slurry, the weight ratio of described salt slurry and potassium felspar sand is 0.001～0.5:1.
3. treatment process according to claim 1 and 2, is characterized in that: described step 3), Reaktionsofen is that suspension preheating burns stove, and maturing temperature is 800～1200 ℃, and roasting time is 30～90min.
4. treatment process according to claim 3, is characterized in that: the leaching liquid described step 4) is evaporated waste ammonia liquid.
5. treatment process according to claim 4, is characterized in that: in described step 7), in the molten reactor of alkali, be sodium hydroxide solution.
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| CN201310430904.3A CN103664242B (en) | 2013-09-18 | 2013-09-18 | Caustic sludge treatment method |
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| CN201310430904.3A CN103664242B (en) | 2013-09-18 | 2013-09-18 | Caustic sludge treatment method |
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| CN103664242B CN103664242B (en) | 2015-07-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016019774A1 (en) * | 2014-08-06 | 2016-02-11 | 华南理工大学 | Method for preparing chlorine-removal alkali residue mixture by utilizing alkali residues through ammonia-soda process and application thereof |
| CN107512721A (en) * | 2016-06-16 | 2017-12-26 | 广州凌玮科技股份有限公司 | It is a kind of that the production method of macro porous silica gel is prepared as raw material using the potassium feldspar white residue that gives up |
| CN112279276A (en) * | 2020-10-13 | 2021-01-29 | 宜兴市宏丰化肥有限公司 | Agricultural harmless treatment process for industrial byproduct potassium salt |
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| KR930009722B1 (en) * | 1991-02-21 | 1993-10-09 | 대한광업 진흥공사 | Iron stone refining method |
| CN1261601A (en) * | 1999-11-19 | 2000-08-02 | 乔希海 | Process for producing potassium chloride from alkaline slag and potassium feldspar |
| CN1298838A (en) * | 1999-12-04 | 2001-06-13 | 乔希海 | Process for preparing potassium chloride from alkali dregs and rock containing potassium |
| CN1298848A (en) * | 2001-01-17 | 2001-06-13 | 刘世永 | Process for preparing K fertilizer from non-soluble potassium ore and waste ammonia-soda solution |
| CN1718555A (en) * | 2004-07-11 | 2006-01-11 | 乔希海 | Method of manufacturing cement |
| CN101857467A (en) * | 2010-05-20 | 2010-10-13 | 广东南方碱业股份有限公司 | Process method for preparing potassic fertilizer by reaction of ammonia evaporation wastewater in soda plant and potash feldspar |
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- 2013-09-18 CN CN201310430904.3A patent/CN103664242B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930009722B1 (en) * | 1991-02-21 | 1993-10-09 | 대한광업 진흥공사 | Iron stone refining method |
| CN1261601A (en) * | 1999-11-19 | 2000-08-02 | 乔希海 | Process for producing potassium chloride from alkaline slag and potassium feldspar |
| CN1298838A (en) * | 1999-12-04 | 2001-06-13 | 乔希海 | Process for preparing potassium chloride from alkali dregs and rock containing potassium |
| CN1298848A (en) * | 2001-01-17 | 2001-06-13 | 刘世永 | Process for preparing K fertilizer from non-soluble potassium ore and waste ammonia-soda solution |
| CN1718555A (en) * | 2004-07-11 | 2006-01-11 | 乔希海 | Method of manufacturing cement |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016019774A1 (en) * | 2014-08-06 | 2016-02-11 | 华南理工大学 | Method for preparing chlorine-removal alkali residue mixture by utilizing alkali residues through ammonia-soda process and application thereof |
| CN107512721A (en) * | 2016-06-16 | 2017-12-26 | 广州凌玮科技股份有限公司 | It is a kind of that the production method of macro porous silica gel is prepared as raw material using the potassium feldspar white residue that gives up |
| CN112279276A (en) * | 2020-10-13 | 2021-01-29 | 宜兴市宏丰化肥有限公司 | Agricultural harmless treatment process for industrial byproduct potassium salt |
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