CN102372377B - Method for advanced treatment of mercury-containing wastewater - Google Patents
Method for advanced treatment of mercury-containing wastewater Download PDFInfo
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- CN102372377B CN102372377B CN 201110282951 CN201110282951A CN102372377B CN 102372377 B CN102372377 B CN 102372377B CN 201110282951 CN201110282951 CN 201110282951 CN 201110282951 A CN201110282951 A CN 201110282951A CN 102372377 B CN102372377 B CN 102372377B
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Abstract
The invention relates to a method for treating mercury-containing wastewater. The method comprises the following steps of: collecting the mercury-containing wastewater to a PH regulating reservoir; adjusting the PH value to be 9-11; pumping the mercury-containing wastewater into a reaction tank by a conveying pump; meanwhile, adding a Na2S solution in the reaction tank and fully reacting; adding a flocculating agent F<3+>; naturally precipitating the generated HgS flocculent precipitate; filtering the reacted supernate by a sand filter tank and enabling the filtered mercury-containing wastewater to feed into an advanced treatment device; feeding the precipitated HgS precipitate into a sludge concentrated tank and concentrating the precipitated HgS precipitate; and feeding the concentrated precipitate into a solid-liquid separating device for solid-liquid separation. According to the invention, the problem that pollution to the environment due to poor treatment effect of the mercury-containing wastewater caused by a synthetic work procedure for producing a polyvinyl chloride resin industrial furnace by adopting a current carbide method is solved; the invention has the advantages of simple and reasonable process, easiness for implementation, quick effect and the like; and the method can be widely applied to the treatment of the mercury-containing wastewater and is especially suitable for the advanced treatment of the mercury-containing wastewater in the production process of the polyvinyl chloride resin.
Description
Technical field:
The present invention relates to a kind for the treatment of process of mercury-containing waste water, particularly be applicable to the method that the mercury-containing waste water in polyvinyl chloride resin production is processed.
Background technology:
Widespread use due to polyvinyl chloride, and the very abundant and carbide acetylene method Technology of China's calcium carbide resource is increasingly mature, make generated by polyvinyl chloride by calcium carbide industry fast development, yet also brought serious problem of environmental pollution when bringing great economic benefit, due to HgCl
2As catalyzer, inevitably cause the passage of mercury, the mercury pollution problem that thereupon causes also is on the rise.Although the harm of mercury-containing waste water is familiar with by people already, and has developed a lot of methods and processed, the processing data in most of document is the result of laboratory or pilot scale research, is actually used in the engineering practice that in industry, mercury-containing waste water is processed still immature.
Announced " a kind of three sections continuous processings are processed the method for mercury-containing waste water " in Chinese patent CN 102010086A, its method is: mercury-containing waste water PH is adjusted to 9-11, is squeezed in retort by pump, add Hg: Na simultaneously in retort
2The mass concentration ratio of S=1: 5-1: 20, mass concentration is the sinking agent Na of 0.5-0.6
2S solution fully reacts, and then adding mass concentration is the inorganic flocculating agent of 0.01-0.03, and the HgS flocks natural sedimentation of generation is got off, and supernatant liquor reaches emission standard after filtering, the HgS throw out decontamination mud thickener after precipitation.But the mercury that still contains lower concentration in the method processed waste water can impact environment.
Summary of the invention:
Thereby the invention reside in the mercury-containing waste water poor processing effect that has solved present calcium carbide route production polyvinyl chloride (PVC) RESINS industrial furnace synthesis procedure generation and cause the problem of environmental pollution, and then a kind of Hg is provided
2+Process thoroughly, pollute little, technique advantages of simple, easily implement, the method for the advanced treatment of mercury-containing wastewater of instant effect.
The technical solution used in the present invention is: a kind of method of advanced treatment of mercury-containing wastewater, comprise PH equalizing tank, transferpump, retort, the sludge thickener that is connected successively and the equipment for separating liquid from solid of processing mercury-containing sludge, it is characterized in that: be provided with the advanced treatment apparatus of sandfiltration pot and mercury-containing waste water after retort, step is as follows:
(1) at first mercury-containing waste water is collected to the PH equalizing tank, PH is adjusted to 9-11;
(2) squeezed in retort by transferpump, add Na simultaneously in retort
2S solution fully reacts, and then adds flocculation agent Fe
3+, the HgS flocks natural sedimentation of generation is got off;
(3) reacted supernatant liquor enters the advanced treatment apparatus of mercury-containing waste water after sandfiltration pot filters,
(4) the HgS throw out decontamination mud thickener after the precipitation enters equipment for separating liquid from solid and carries out solid-liquid separation after sludge thickener is concentrated, the liquid after separation returns to the PH equalizing tank, and the solid barrelling sealing after separation is collected.
The method of described a kind of advanced treatment of mercury-containing wastewater, the advanced treatment apparatus of mercury-containing waste water comprise reduction reactor and the wet cyclone that is connected successively; The uniform and stable flow velocity of mercury-containing waste water after sandfiltration pot filters is sent into reduction reactor, filler in reduction reactor is metallic zinc, mercury ion in reduction reactor in mercury-containing waste water and metallic zinc generation reduction reaction, separate out liquid mercury simple substance and enter together with waste water after reduction and carry out liquid liquid in wet cyclone and separate, mercury simple substance after separating is discharged by the bottom of wet cyclone and the barrelling sealing is collected, supernatant liquor after separation by the top of wet cyclone out discharges after mercurous concentration≤0.5 μ g/l.Use the zinc granule reductive agent can make mercury ion be reduced into mercury metal, and reductive agent is cheap, loses less in solvent, removal of mercury efficient is high, is conducive to the processing of mercury-containing waste water.
The method of described a kind of advanced treatment of mercury-containing wastewater, connect an adsorber after wet cyclone, filler in adsorber is molecular sieve, supernatant liquor after the separation out of wet cyclone top enters adsorber, unreacted mercury ion is adsorbed the molecular sieve adsorption in device in reduction reactor, discharges after the mercurous concentration of waste water after absorption≤0.5 μ g/l.Molecular sieve has stronger removal effect to divalence mercury, and larger loading capacity arranged, can use in the wider scope of reaction conditions (mercury concentration, PH, temperature, duration of contact etc.), technological process is easy to control, easy enforcement, is conducive to further improve the processing efficiency of mercury-containing waste water.
The method of described a kind of advanced treatment of mercury-containing wastewater, one waste water circulation pump is set after adsorber, waste water after absorption is sent waste water into reduction reactor by the waste water circulation pump with uniform and stable flow velocity again and is carried out reduction reaction, carrying out liquid liquid through wet cyclone separates, supernatant liquor after the separation out of wet cyclone top enters adsorber again, discharges after the mercurous concentration of the supernatant liquor after separation≤0.5 μ g/l.
The method of described a kind of advanced treatment of mercury-containing wastewater, adsorber top connection one Gas Phase Adsorption device is filled with gac in the Gas Phase Adsorption device.Use gac, be conducive to the mercury in gas phase is adsorbed onto in gac, reached the purpose of protection of the environment.
The method of described a kind of advanced treatment of mercury-containing wastewater, molecular sieve are reproducible, when molecular sieve reach absorption saturated after, pass into steam in adsorber bottom molecular sieve regenerated, by discharging after mercuryvapour enters the Gas Phase Adsorption device containing of molecular sieve.Utilize the steam waste heat in chemical process that molecular sieve is regenerated, but effective use of energy sources reduce production costs, reached the purpose of protection of the environment.
Filler in the method for described a kind of advanced treatment of mercury-containing wastewater, adsorber is 13X type molecular sieve, 5A type molecular sieve or solid activated carbon, the heavy metal chelate resin of spherical or column.Wherein 13X and 5A represent respectively the model of molecular sieve, and its aperture is respectively 10A and 5A.
Filler in the method for described a kind of advanced treatment of mercury-containing wastewater, reduction reactor is metal, and the electropotential of its ionic state is lower than the electropotential of mercury ion.
Filler in the method for described a kind of advanced treatment of mercury-containing wastewater, reduction reactor is metallic zinc, metallic iron or the metallic aluminium of the spherical or column of 5-20mm.
The method of described a kind of advanced treatment of mercury-containing wastewater, uniform and stable flow velocity are 4-15m
3/ h.
The present invention is in line with the purpose of protection of the environment, energy-saving and emission-reduction, the factor that is difficult to process this contaminate environment for the mercury-containing waste water of calcium carbide route production polyvinyl chloride (PVC) RESINS industrial furnace synthesis procedure generation, by the treatment process of chemical precipitation method, metallic reducing and molecular sieve adsorption filtration, thereby treated mercury-containing waste water can be reached≤0.5 μ g/l; Adopt chemical reaction method to process the high density mercury-containing waste water, utilize mercury ion to generate the principle of the precipitation that is insoluble in water with sulfide, make Hg
2+Be converted into HgS, by adding flocculation agent, the HgS natural subsidence got off; Then adopt metal deoxidization to process the lower concentration mercury-containing waste water, its speed of reaction is higher, can directly reclaim mercury metal; and the final barrelling sealing of the mercury metal after separating is collected; adopt the method for molecular sieve adsorption, because molecular sieve has larger loading capacity, can use in the wider scope of reaction conditions; and molecular sieve is renewable; therefore reusable, prevent secondary pollution, and then reach the purpose of protection of the environment; simultaneously also reduce production cost, improved economic benefit.One aspect of the present invention makes mercury-containing waste water process thoroughly, pollute little; On the other hand because filler in native system is reusable, invest littlely, easily implement; Technique advantages of simple simultaneously can effectively reach the purpose of energy-saving and emission-reduction, protection of the environment.The present invention can be widely used in being specially adapted in the advanced treatment of the mercury-containing waste water in polyvinyl chloride resin production in the processing of mercury-containing waste water.
Description of drawings:
Fig. 1 is the embodiments of the invention process flow sheet;
In Fig. 1: 1 is that retort, 2 is that transferpump, 3 is that PH equalizing tank, 4 is that sludge thickener, 5 is that equipment for separating liquid from solid, 6 is that reduction reactor, 7 is that wet cyclone, 8 is that adsorber, 9 is that Gas Phase Adsorption device, 10 is that waste water circulation pump, 11 is sandfiltration pot.
Embodiment:
In accompanying drawing 1, the present embodiment comprises the steps: to comprise PH equalizing tank 3, transferpump 2, retort 1, the sludge thickener 4 that is connected successively and the equipment for separating liquid from solid 5 of processing mercury-containing sludge, be provided with the advanced treatment apparatus of sandfiltration pot 11 and mercury-containing waste water after retort, step is as follows: at first mercury-containing waste water is collected to the PH equalizing tank, PH is adjusted to 9-11; Squeezed in retort by transferpump, add Na simultaneously in retort
2S solution fully reacts, and then adds flocculation agent Fe
3+, the HgS flocks natural sedimentation of generation is got off; Reacted supernatant liquor enters the advanced treatment apparatus of mercury-containing waste water after sandfiltration pot filters, HgS throw out decontamination mud thickener after precipitation, enter equipment for separating liquid from solid and carry out solid-liquid separation after sludge thickener is concentrated, liquid after separation returns to the PH equalizing tank, and the solid barrelling sealing after separation is collected.
Another embodiment difference is that the advanced treatment apparatus of mercury-containing waste water comprises reduction reactor 6 and the wet cyclone 7 that is connected successively; The uniform and stable flow velocity of mercury-containing waste water after sandfiltration pot filters is sent into reduction reactor, filler in reduction reactor is metallic zinc, mercury ion in reduction reactor in mercury-containing waste water and metallic zinc generation reduction reaction, separate out liquid mercury simple substance and enter together with waste water after reduction and carry out liquid liquid in wet cyclone and separate, mercury simple substance after separating is discharged by the bottom of wet cyclone and the barrelling sealing is collected, supernatant liquor after separation by the top of wet cyclone out discharges after mercurous concentration≤0.5 μ g/l.
Another embodiment difference is to connect an adsorber after wet cyclone, filler in adsorber is molecular sieve, supernatant liquor after the separation out of wet cyclone top enters adsorber, unreacted mercury ion is adsorbed the molecular sieve adsorption in device in reduction reactor, discharges after the mercurous concentration of waste water after absorption≤0.5 μ g/l.
Another embodiment difference is after adsorber, a waste water circulation pump to be set, waste water after absorption is sent waste water into reduction reactor by the waste water circulation pump with uniform and stable flow velocity again and is carried out reduction reaction, carrying out liquid liquid through wet cyclone separates, supernatant liquor after the separation out of wet cyclone top enters adsorber again, discharges after the mercurous concentration of the supernatant liquor after separation≤0.5 μ g/l.
Another embodiment difference is adsorber top connection one Gas Phase Adsorption device, is filled with gac in the Gas Phase Adsorption device.
Another embodiment difference is that molecular sieve is reproducible, when molecular sieve reach absorption saturated after, pass into steam in adsorber bottom molecular sieve regenerated, by discharging after mercuryvapour enters the Gas Phase Adsorption device containing of molecular sieve.
Another embodiment difference is that the filler in adsorber is spherical 13X type molecular sieve.
Another embodiment difference is that the filler in adsorber is the 5A type molecular sieve of column.
Another embodiment difference is that the filler in reduction reactor is the metallic zinc of 10mm column.
Another embodiment difference is that the filler in reduction reactor is the spherical metallic aluminium of 5mm.
Another embodiment difference is that uniform and stable flow velocity is 5m
3/ h.
Another embodiment difference is that uniform and stable flow velocity is 15m
3/ h.
Be below workflow of the present invention and principle:
the mercurous waste hydrochloric acid that produces in producing from generated by polyvinyl chloride by calcium carbide, the mercury-containing waste waters such as waste lye, be collected to the PH equalizing tank, regulate its PH and be adjusted to 9-11, squeezed in retort by transferpump, simultaneously add heavy metal settling agent fully to react in retort, and then add inorganic flocculating agent, the HgS flocks natural sedimentation that generates is got off, the supernatant liquor that produces, after filtering, sandfiltration pot enters reduction reactor, the metallic zinc generation reduction reaction that mercury ion in reduction reactor in mercury-containing waste water and reactor are loaded, separating out liquid mercury simple substance enters together with waste water after reduction and carries out liquid liquid in wet cyclone and separate, mercury simple substance after separating is discharged and the barrelling sealing by the bottom of wet cyclone, supernatant liquor after separation out enters adsorber again by the top of wet cyclone, unreacted mercury ion is adsorbed the adsorbent of molecular sieve absorption in device in reduction reactor, then the waste water after absorption again by the waste water circulation pump waste water after with underproof absorption send into again reduction reactor and continue circulating reaction, and guarantee uniform and stable circular flow, until the mercury-containing waste water concentration of waste water circulation pump discharge lower than 0.005ppm after, open the valve of pump discharge, waste water is sent into composite wastewater treatment plant of full factory to be processed.The mercury-containing sludge that settles down in retort flows automatically and enters sludge thickener, arrive equipment for separating liquid from solid by sludge pump again, gained filtrate is returned to the PH equalizing tank, the sedimentation removal of mercury that circulates reaction, the gained filter cake leaves the useless storehouse of danger in, unification is transported, thereby reaches the purpose of removal of mercury environmental contamination reduction.
After molecular sieve adsorption reaches capacity, pass into steam from the bottom and carry out regenerative process, top mercurous gas out enters the Gas Phase Adsorption device by charcoal absorption, thereby reaches the purpose of protection of the environment.
Claims (5)
1. the method for an advanced treatment of mercury-containing wastewater, comprise pH regulator pond, transferpump, retort, the sludge thickener that is connected successively and the equipment for separating liquid from solid of processing mercury-containing sludge, it is characterized in that: be provided with the advanced treatment apparatus of sandfiltration pot and mercury-containing waste water after retort, step is as follows:
(1) at first mercury-containing waste water is collected to the pH regulator pond, with pH regulator to 9-11;
(2) squeezed in retort by transferpump, add Na simultaneously in retort
2S solution fully reacts, and then adds flocculation agent Fe
3+, the HgS flocks natural sedimentation of generation is got off;
(3) reacted supernatant liquor enters the advanced treatment apparatus of mercury-containing waste water after sandfiltration pot filters,
(4) the HgS throw out decontamination mud thickener after the precipitation enters equipment for separating liquid from solid and carries out solid-liquid separation after sludge thickener is concentrated, the liquid after separation returns to the pH regulator pond, and the solid barrelling sealing after separation is collected;
The advanced treatment apparatus of mercury-containing waste water comprises reduction reactor and the wet cyclone that is connected successively; The uniform and stable flow velocity of mercury-containing waste water after sandfiltration pot filters is sent into reduction reactor, filler in reduction reactor is metallic zinc, mercury ion in reduction reactor in mercury-containing waste water and metallic zinc generation reduction reaction, separate out liquid mercury simple substance and enter together with waste water after reduction and carry out liquid liquid in wet cyclone and separate, mercury simple substance after separating is discharged by the bottom of wet cyclone and the barrelling sealing is collected, supernatant liquor after separation by the top of wet cyclone out, qualified rear qualified discharge;
Connect an adsorber after wet cyclone, filler in adsorber is molecular sieve, supernatant liquor after the separation out of wet cyclone top enters adsorber, and unreacted mercury ion is adsorbed the molecular sieve adsorption in device in reduction reactor, the qualified rear qualified discharge of the waste water after absorption;
One waste water circulation pump is set after adsorber, waste water after absorption is sent waste water into reduction reactor by the waste water circulation pump with uniform and stable flow velocity again and is carried out reduction reaction, carrying out liquid liquid through wet cyclone separates, supernatant liquor after the separation out of wet cyclone top enters adsorber again, the qualified rear qualified discharge of the supernatant liquor after separation;
The adsorber top connects a Gas Phase Adsorption device, is filled with gac in the Gas Phase Adsorption device.
2. the method for a kind of advanced treatment of mercury-containing wastewater according to claim 1, it is characterized in that: molecular sieve is reproducible, when molecular sieve reach absorption saturated after, pass into steam bottom adsorber molecular sieve is regenerated, by discharging after mercuryvapour enters the Gas Phase Adsorption device containing of molecular sieve.
3. the method for a kind of advanced treatment of mercury-containing wastewater according to claim 2 is characterized in that: the filler in adsorber is 13X type molecular sieve, the 5A type molecular sieve of spherical or column.
4. the method for a kind of advanced treatment of mercury-containing wastewater according to claim 1 is characterized in that: the filler in reduction reactor is the metallic zinc of the spherical or column of 5-20mm.
5. the method for a kind of advanced treatment of mercury-containing wastewater according to claim 1, it is characterized in that: described uniform and stable flow velocity is 4-15m
3/ h.
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| US4565633A (en) * | 1984-05-08 | 1986-01-21 | Harza Engineering Company | Removal of dissolved heavy metals from aqueous waste effluents |
| US8034246B2 (en) * | 2007-05-16 | 2011-10-11 | Exxonmobil Research & Engineering Company | Wastewater mercury removal process |
| CN102001734B (en) * | 2010-12-01 | 2013-06-12 | 新疆天业（集团）有限公司 | Heavy metal settling agent for treating mercury-containing wastewater |
| CN102010086B (en) * | 2010-12-01 | 2013-01-09 | 新疆天业（集团）有限公司 | Method for treating mercury-containing wastewater with three-section continuous process |
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Effective date of registration: 20180224 Address after: No. 36 North Third East Road, the Xinjiang Uygur Autonomous Region Shihezi Development Zone, the Xinjiang Uygur Autonomous Region Co-patentee after: Xinjiang Tianye (Group) Co., Ltd. Patentee after: Tianchen Chemical Co., Ltd. Address before: 832000, No. 36, North East Road, Shihezi economic and Technological Development Zone, the Xinjiang Uygur Autonomous Region Patentee before: Tianchen Chemical Co., Ltd. |