CN101524698A - Caustic sludge dehydration method - Google Patents
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- CN101524698A CN101524698A CN200910068363A CN200910068363A CN101524698A CN 101524698 A CN101524698 A CN 101524698A CN 200910068363 A CN200910068363 A CN 200910068363A CN 200910068363 A CN200910068363 A CN 200910068363A CN 101524698 A CN101524698 A CN 101524698A
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Abstract
The invention relates to a caustic sludge dehydration method which comprises the steps: 1) the caustic sludge is processed by coarse grinding and mixed with solvent having the mass ratio of 1-1.5; the mixture is put into a stainless steel high-pressure autoclave and slowly charged with air to be pressurized to 5-10MPa, and the leak tightness of the high-pressure autoclave is checked; 2) when the gas in the high-pressure autoclave is completely emptied and equipment are examined to have no leakage phenomenon, the caustic sludge is dehydrated under the conditions that the temperature raises to 150-240 DEG C, the pressure is 1-3.0MPa, the time is 2-4h, and the rotating speed is 100-180r/min; 3) after the reaction, a heating jacket is dismounted, and the temperature is reduced to be the room temperature; the cooling water is continuously added to accelerate the cooling rate; after the high-pressure autoclave is cooled to be the room temperature naturally and the pressure is zero, the residual liquid in the high-pressure autoclave is collected as well as pumped and filtered repeatedly; finally, the caustic sludge is recovered. The invention can be used for achieving the aim of dehydration with a shorter time, and the technical operation process is simple, easy to implement and in accordance with the principle of solid waste resource utilization; the caustic sludge which is dehydrated can be used for other purposes, and the dehydration rate of the caustic sludge reaches up to 78.37%.
Description
Technical field
The invention belongs to the chemical industry for making chlorine and alkali technical field, relate to a kind of method of caustic sludge dehydration that the waste residue of soda ash process discharging is produced in ammonia-soda process.
Background technology
The disadvantage that soda ash is produced in ammonia-soda process is can produce a large amount of discarded objects in the ammonia distillation process flow process.According to statistics, every production 1t soda ash will be discharged 9～11m
3Discarded object, wherein contain the about 0.3～0.6t of solid slag.China have now Dalian, Tianjin, Qingdao three big ammonia alkali factories all be located in coastal, produce mainly be for many years store up by building a dam, vacant lot stores up, waste clear solution row sea and mix the extra large way of the row waste residue that disposes waste liquid.Along with the continuous development of producing, the waste discharge amount increases year by year in recent years, and original waste discharge facility can not satisfy the production needs.As Tianjin Caustic Soda Plant the liquid and waste slag produced salt flat vacant lot that utilizes is stored up, the clear liquid after sinking clearly naturally flows into the Bohai Sea, and pile up like a mountain for the waste residue through accumulating for many years, form two " lime low banks between fields ", floor space has reached more than 350 hectare, and large stretch of salt pan not only accounts for, the danger of landslide is arranged simultaneously, become public hazards.The original extra large Ba Zhachang of Dalian chemical company fills up, and it is excessive that the waste liquid that suspends is in a large number got over the dam, causes discharging of waste liquid to exceed standard, and the waste residue deposition is silted the serious consequence in navigation channel up.Along with environmental problem becomes the problem that the whole world faces jointly gradually, some developed countries have closed ammonia-soda process soda plant successively, and China is a developing country, and it is unpractical closing such alkali factory.The strategy of sustainable development is the elementary tactics of China, so effective improvement of the three wastes and utilization are one of important measures of protection environment.
From the generative process of alkaline residue as can be seen: alkaline residue is lime stone and the byproduct of crude salt after specific flow process.Main water insoluble active ingredient is CaCO
3, Mg (OH)
2, CaSO
4, also contain a spot of Al
2O
3, Fe
2O
3, SiO
2, content is 60%～80%; And the salt main component of ease of solubility is CaCl
2, NaCl etc., content is 12%～22%; In addition, also contain 6%～10% acid non-soluble substance.The lyotropic salt chemical analysis shows that alkaline residue is alkalescence, and the pH value of alkaline residue is generally 10～12.
Soluble chloride (CaCl in the alkaline residue
2, NaCl) salt content is higher, promptly chloride ion content is higher.By quiet molten and leaching test to alkaline residue, analyze the precipitation process of chlorion in the leachate, find that an alkaline residue stacking rising to the underground water chlorine ion concentration has very big influence.Jiaozuo City was the water quality variation year by year of two, seven water-supply plants of source water with deep layer karst water, and the chlorine ion concentration of two water factories is elevated to 119mg/L in 2003 by 58.7mg/L in 1996; And the chlorion of the beverage well of hydrological team of mineral bureau is increased to 1490mg/L in 2003 by 86mg/L in 1998 especially, because chlorine ion concentration raises, has also caused the increase of cations in the water, thereby has caused the rising of underground water total hardness.
Pointing out that the particle of alkaline residue is very tiny in " the engineering property research of caustic sludge soil " of the prosperous grade of intercalation timely rain, is another principal character of alkaline residue.Wherein, alkaline residue particle diameter＜10 of (volume fraction) micron (being equivalent to 1250 orders) more than 65%, the alkaline residue more than 95%＜25 micron (being equivalent to 500 orders), the maximum particle diameter of alkaline residue is 38 microns (being equivalent to 320 orders).Because the fine size of alkaline residue, specific area is big, has colloidal nature, so its powder granule sinking speed is slow, and the moisture content height, is difficult to dehydration, and this is a difficult point of dreg control.
Yao De and Lou Xingyi etc. point out in " alkaline residue (white clay) comprehensive utilization " and " discussion of alkaline residue (white clay) comprehensive Utilization Ways " respectively: be earth work such as reclaim fields from the sea, build the road aspect the alkaline residue consumption maximum, its natural moisture content height, a large amount of airings is very difficult, in the process of filling, also be difficult to control water content finely, may be present in the bigger scope.At present, but the Finland LAROX public affairs PF full automatic pressure filter that Tianjin Caustic Soda Plant introduces can meet the demands, home equipment is difficult to be competent at.Should only not work hard to this problem, seek new method and develop the caustic sludge dehydration technology from dehydration equipment.
Qiao Xihai " drying means of alkaline residue " has invented and has isolated dry method: with storing caustic sludge or directly discharge the alkaline residue of dreg liquid after deposition, press filtration to be placed on air dry to water content on the natural ground that has separation layer be 20～40% the block plain ash of alkaline residue.Wang Hongbo etc. " the alkaline residue hydrophobic modified research in surface " have studied alkaline residue surface hydrophobic by the mechanochemical modification method and have handled, with the calcium stearate is modifier, as index, having carried out with the activation alkaline residue is the lyotropic salt and the test of chlorion stripping property of the asphalt of filler preparation with dispersion rate and activation index.Adopt single physics or chemical method to be difficult to obtain advanced reasonably technical-economic index, the stacking that changes this solid waste causes the problem of water pollution then, and control measures must be able to consume a large amount of alkaline residues, technically want simple and feasible and certain economic benefits is arranged.
Summary of the invention
Under field conditions (factors), always moisture in the alkaline residue.Be present in the lattice frame of alkaline residue water inner or that participate in the alkaline residue structure and be called in conjunction with water, it only just can turn to vaporous water under than higher temperature and separate with alkaline residue.Free water is to be present in alkaline residue surface field coverage water in addition, has solvability, can transmit hydrostatic pressure.
The mineral grain surface generally has negative electrical charge.In the surface of close alkaline residue, electrostatic attraction is the strongest, and it forms fixed bed to ion hydration and firm being adsorbed on the alkaline residue surface of polar molecule.In the periphery of fixed bed, electrostatic attraction is smaller, so the activity of ion hydration and polar water molecules forms diffusion layer than big in fixed bed.So can be divided into again by force in conjunction with water and weak in conjunction with two kinds in water, is water in the fixed bed in conjunction with water in conjunction with water by force, weakly then is equivalent to water in the diffusion layer in conjunction with water.By force in conjunction with water be meant near the alkaline residue surface in conjunction with water, it does not have the ability of dissolved salts, can not transmit hydrostatic pressure, could move when having only heat absorption to become steam.Its firm alkaline residue surface that is combined in of this water electrode, its character approaches solid, has great viscosity, elasticity and shearing strength.Particle is thinner, and specific area is bigger, and maximum sorption degree is bigger.Weak is to be close proximity to by force to obtain the peripheral one deck that forms in conjunction with moisture film in conjunction with water in conjunction with water.It still can not transmit hydrostatic pressure, but thicker weak of moisture film can slowly shift to contiguous thin moisture film in conjunction with water.Weak far away from particle in conjunction with water, its electric van der Waals' force that is subjected to is littler, and carries out the transition to Free water gradually.The specific area of alkaline residue (the soil particle total surface area of unit volume or quality) is very big, cause the alkaline residue surface can be very big, the hydrophilic ability of adding carbonate is more intense, therefore alkaline residue has strong suction-operated to water, cause alkaline residue that great hole system and pore water are arranged, this is the very high reason of alkaline residue water content.Under natural stacking states, the alkaline residue water content of native state is up to 260%, and void ratio is greater than 2.97, and porosity n is greater than 75%.
The character such as structure, composition, particle diameter, surface characteristic, charge that to the effect that change alkaline residue by high temperature, high pressure of the present invention reduce its hydrophily, improve hydrophobicity, thereby change alkaline residue sedimentation and strainability.
Technical scheme of the present invention is as follows:
A kind of waste residue dehydration method is characterized in that step is as follows:
1) alkaline residue being carried out coarse crushing, is to join in the stainless steel autoclave after 1～1.5 the solvent with mass ratio, slowly charges into air pressurized to a little more than experimental pressure, checks the sealing of autoclave;
2) treat complete emptying high pressure gas reactor, after checkout facility does not have leakage phenomenon; Being warmed up to 150～240 ℃, pressure is 1～3MPa, time 2～4h, makes caustic sludge dehydration under 100～180r/min rotating speed;
3) after reaction finishes, heating jacket is unloaded, reductions temperature is a room temperature, continues logical cooling water to accelerate cooling rate, treats that autoclave is cooled to after pressure makes zero, and collects that raffinate also carries out suction filtration repeatedly in the still, the recovery alkaline residue.
Described solvent is ethanol, water, chloroform, acetone or ether etc.
Above-mentioned steps 1) part in the alkaline residue of immersion back has become Free water in conjunction with water, and some lyotropic salt is (as CaCl
2With NaCl etc.) meet water-soluble separating, original skeleton is caused to a certain degree destruction.
Above-mentioned steps 2) through behind the certain hour, under the effect of solvent and pore water, various substance crystallizations or be deposited to the surface and the intergranular contact position of particle, volume has increase to a certain degree, this can reduce the void ratio of alkaline residue, and the spacing of particle reduces, and increases packing.
Steam all is in superheat state in the everywhere of autoclave, thereby heat can be supplied with the moisture in the alkaline residue, takes away steam simultaneously.Overheated steam is circulation continuously in system, simultaneously continuously discharges superfluous steam so that keep pressure in the system.The superheated steam surface temperature is high, and dewatering time reduces, and has reduced the bulk density of alkaline residue, has reduced great retention charge usefulness, has also avoided alkaline residue to stack simultaneously and has caused the karstic ground water chloride ion contamination.Because steam is slightly overheated, the requirement of having avoided heating a large amount of air, solvent is easy to get in addition, thereby causes energy-conservation.The discharge capacity of alkaline residue is big, need remove a large amount of moisture, and wet amount of dividing is bigger, and efficient improves bigger, and this has just given its economical efficiency of scale.The present invention can reach the dehydration purpose in the short period of time, simple, the easily enforcement of technical operating procedure, and meet the principle that solid waste resource recovery utilizes, the alkaline residue after the treated dehydration can be done his and use.With respect to dewatering in air ambient, the method has whole positive roles.The caustic sludge dehydration rate is more than 50%.
The specific embodiment
Example 1: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, absolute ethyl alcohol 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 3.0MPa, 210 ℃ of temperature, rotating speed 100r/min, heating 2h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 76.84g, the alkaline residue color is bleached by ash behind the air dry 3d, weigh again once 39.76g.The caustic sludge dehydration rate is 60.24%.
Example 2: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, absolute ethyl alcohol 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.0MPa, 150 ℃ of temperature, rotating speed 100r/min, heating 2h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 80.18g, the alkaline residue color is bleached by ash behind the air dry 3d, weigh again once 49.24g.The caustic sludge dehydration rate is 50.76%.
Example 3: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 3.0MPa, 240 ℃ of temperature, rotating speed 100r/min, heating 2h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 69.05g, the alkaline residue color is bleached by ash behind the air dry 3d, weigh again once 30.97g.The caustic sludge dehydration rate is 69.03%.
Example 4: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 3.0MPa, 240 ℃ of temperature, rotating speed 150r/min, heating 2h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 57.50g, the alkaline residue color is bleached by ash behind the air dry 3d, weigh again once 24.08g.The caustic sludge dehydration rate is 75.92%.
Example 5: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 210 ℃ of temperature, rotating speed 150r/min, heating 2h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 71.25g, the alkaline residue color is bleached by ash behind the air dry 3d, weigh again once 39.53g.The caustic sludge dehydration rate is 60.47%.
Example 6: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 210 ℃ of temperature, rotating speed 150r/min, heating 3h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 69.54g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 28.13g.The caustic sludge dehydration rate is 71.87%.
Example 7: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, ether 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 210 ℃ of temperature, rotating speed 150r/min, heating 4h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 67.78g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 22.73g.The caustic sludge dehydration rate is 77.27%.
Example 8: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 210 ℃ of temperature, rotating speed 180r/min, heating 4h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 63.84g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 21.63g.The caustic sludge dehydration rate is 78.37%.
Example 9: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, chloroform 100g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 210 ℃ of temperature, rotating speed 150r/min, heating 4h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 66.04g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 42.80g.The caustic sludge dehydration rate is 57.20%.
Example 10: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, running water 130g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 2MPa, 210 ℃ of temperature, rotating speed 150r/min, heating 4h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 65.28g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 25.68g.The caustic sludge dehydration rate is 74.32%.
Example 11: wash autoclave inwall, stirring and composition surface repeatedly with distilled water, dip in ethanol with cotton or silk again and clean.Get the clean beaker of a 300mL, on electronic balance, accurately take by weighing alkaline residue 100g, acetone 150g, join in the autoclave.Feed intake after the end, with lens paper wiping autoclave face sealing place gently, close the lid, tighten up a screw symmetrically with the torque spanner across, progressively afterburning symmetry tightens.Behind the leak test air in the still is drained, make earlier and stir switch, speed governing heater switch set to zero, drive the console current switch again.Setting pressure 1.5MPa, 200 ℃ of temperature, rotating speed 150r/min, heating 4h.Reaction is finished and is stopped to stir, and residual gas in the still is drained, and turns on screw sampling suction filtration.On electronic balance, weigh then 65.82g, put into 100 ℃ of dry 12h of baking oven after the alkaline residue color bleach by ash, weigh again once 45.32g.The caustic sludge dehydration rate is 54.68%.
The method of a kind of caustic sludge dehydration that the present invention proposes, be described by embodiment, person skilled obviously can be changed or suitably change and combination preparation method as herein described in not breaking away from content of the present invention, spirit and scope, realizes technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (2)
1. the method for a caustic sludge dehydration is characterized in that step is as follows:
1) alkaline residue being carried out coarse crushing, is to join in the stainless steel autoclave after 1～1.5 the solvent with mass ratio, slowly charges into air a little more than test pressure, checks the sealing of autoclave;
2) treat complete emptying high pressure gas reactor, after checkout facility does not have leakage phenomenon; Being warmed up to 150～240 ℃, pressure is 1～3.0MPa, time 2～4h, makes caustic sludge dehydration under 100～180r/min rotating speed;
3) after reaction finishes, heating jacket is unloaded, reductions temperature is a room temperature, continues logical cooling water to accelerate cooling rate, treats that autoclave is cooled to after pressure makes zero, and collects that raffinate also carries out suction filtration repeatedly in the still, the recovery alkaline residue.
2. a kind of waste residue dehydration method as claimed in claim 1 is characterized in that described solvent is ethanol, water, chloroform, acetone or ether.
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| CN200910068363A CN101524698A (en) | 2009-04-03 | 2009-04-03 | Caustic sludge dehydration method |
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|---|---|---|---|
| CN200910068363A CN101524698A (en) | 2009-04-03 | 2009-04-03 | Caustic sludge dehydration method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113069709A (en) * | 2021-03-30 | 2021-07-06 | 北京荣创岩土工程股份有限公司 | Treatment process for stably dehydrating ammonia-soda process alkaline residue |
| CN115463950A (en) * | 2022-09-13 | 2022-12-13 | 昆明理工大学 | High-pressure dehydration method for water-containing material |
-
2009
- 2009-04-03 CN CN200910068363A patent/CN101524698A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113069709A (en) * | 2021-03-30 | 2021-07-06 | 北京荣创岩土工程股份有限公司 | Treatment process for stably dehydrating ammonia-soda process alkaline residue |
| CN115463950A (en) * | 2022-09-13 | 2022-12-13 | 昆明理工大学 | High-pressure dehydration method for water-containing material |
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