CN102942211A - Method for recycling mercury from mercury-containing solid wastes - Google Patents
Method for recycling mercury from mercury-containing solid wastes Download PDFInfo
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- CN102942211A CN102942211A CN2012104674818A CN201210467481A CN102942211A CN 102942211 A CN102942211 A CN 102942211A CN 2012104674818 A CN2012104674818 A CN 2012104674818A CN 201210467481 A CN201210467481 A CN 201210467481A CN 102942211 A CN102942211 A CN 102942211A
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Abstract
The invention discloses a method for recycling mercury from mercury-containing solid wastes. The method comprises the following steps: introducing N2 (or other inert gases) into mercury-containing wastes at 100 DEG C-200 DEG C and drying for 0.5-10 hours; introducing the chlorine at 200 DEG C-400 DEG C for chlorinating for 0.5-10 hours; introducing N2 again at 400 DEG C-750 DEG C and dry distilling for 1-10 hours; and lastly, washing with a solvent, thereby obtaining a product, and meanwhile, absorbing the dry distilling tail gas by using absorption liquid. According to the method, the recovery rate of the mercury can reach 80-99%; the recycled waste mercury bichloride contact agent carrier is not damaged; the mercury content is extremely reduced to below 0.1% and the recycled waste mercury bichloride contact agent carrier still can be applied to the production of a mercury bichloride contact agent; the pollution problem of the mercury-containing waste and the recycling problem of the mercury resource are solved according to the method; the traditional mercury recycling method and the mercury bichloride production are integrated; the production cost is saved; and the method has the advantages of zero remnant of waste residue and waste water, simpleness in technology, low cost, waste recycling and environmental protection.
Description
Technical field
The present invention relates to the comprehensive regulation of mercury-containing wastes and utilize technical field, be particularly useful for the recovery of mercury in the useless mercury catalyst of a kind of acetylene hydrochlorination.
Background technology
Mercury is a kind of argenteous liquid metal, and volatility is very large under the normal temperature, and it is applied in the industrial sectors such as chemical industry and petrochemical industry, pharmacy, paper pulp papermaking, electric appliance and electronic instrument widely, and with " waste gas, waste residue, waste water " three kinds of approach contaminate environment.Wherein waste residue is mainly derived from the useless mercury catalyst that the calcium carbide process PVC industry produces, the nearly 10,000 tons of useless mercury catalysts of the annual generation of whole nation calcium carbide process PVC industry, wherein mercury content reaches 2-5%, so a large amount of mercury-containing wastes has brought huge pressure to environmental protection, conventional processing is to concentrate landfill disposal at present, the pyrometallurgical smelting that other producer adopts reclaims the method for mercury, to give up mercury catalyst through processing such as unslaked lime or caustic soda, make mercury wherein be converted into red precipitate, burn again and aftertreatment therefrom extracts mercury simple substance.Pyrogenic process reclaims the waste that mercury can cause resource, and its recovery added value is lower simultaneously.
Patent CN1125775 discloses by the method that obtains mercury metal in the chloride containing mercurous product, the method can make dimercurion be reduced into Elemental Mercury (zinc) and the metal that forms amalgam exists and to process described product with subacidity and the thermal chlorination thing aqueous solution down, with the mercury of recovery metallic state.Muriate wherein is sodium-chlor and ammonium chloride preferably, strength of solution be 1 mole between the saturation concentration, 2 moles are better; Between 80-100 ℃ of the service temperatures, the mercury of gained can be that 1 mole of Chloride Solution between 1-1.5 washs to purify by the pH value, and finally can obtain weight is 96 grams and the amalgam that contains 84.9 gram mercury.The mercury that the method only relates in the chloride containing mercurous product reclaims, and what obtain is mercury simple substance, its easy volatile so that production security be difficult to guarantee, use and have certain limitation.
Patent CN102115156A discloses the method that a kind of mercurous spent catalyst prepares mercury chloride co-producing sodium chloride and sulfuric acid, the mercury catalyst that will give up makes mercury chloride co-producing sodium chloride and sulfuric acid through following three steps, the mercury catalyst that at first will give up is sent in the sealed distiller and is distilled, make mercury chloride be directly sublimed into gas, be cooled to again the mercury chloride of liquid; Secondly mercuric chloride solution obtained above and sodium sulfide solution are reacted, generate zunsober and sodium-chlor mixing solutions, then obtain the filter cake zunsober through closed suction filtration, generate again mercury chloride and the sulfuric acid mixed solution of precipitation with hydrochloric acid and oxygen reaction, filtration is able to filter cake mercury chloride, through wash drying, crushing packing is finished product mercury chloride; Remaining clarified liq sulfuric acid is sent sodium chloride solution obtained above in the air distillation device at last and is distilled through the concentrated sulfuric acid product that obtains more than 90%, obtains the sodium chloride crystal product; The method step is comparatively complicated, and the wastewater and waste acid of generation needs further to process.
Patent CN101288850A discloses a kind of method of process for oxychlorination regenerated mercuric chloride catalyst, the method is for selecting to get the useless mercuric chleride catalyst of suitable granularity, in blender loader, make activation solution, pump into activator, under 15-40 ℃, normal pressure, soak activation treatment after 30 minutes, soak solution is put into blender loader, in soak solution, pass into 1-3kg chlorine, then pump in the activator, finish an immersion, working cycle; Repeat above-mentioned immersion, working cycle until the soak solution color changes sundown into by the discipline look, then soak solution is put into blender loader, make circulating mother liquor for batching next time; Useless mercuric chloride catalyst after the immersion is made mercuric chloride catalyst after entering the absorption of subsequent processing dipping, drying, cooling as impregnated material.The method is only applicable to the regeneration of useless mercury catalyst, and is not necessarily applicable for other mercurous solid waste.
Summary of the invention
The object of the invention is to solve environmental pollution and the mercury serious waste of resources that causes after the mercurous solid waste landfill disposal, the prior art rate of recovery is low, the problems such as inconvenient operation, and then the recovery method of mercury in a kind of mercurous solid waste is provided, this method is easy to operate, and the rate of recovery is high.
The method that the present invention aims to provide a kind of simple and fast reclaims mercury chloride from mercurous solid waste, especially be fit to reclaim the mercury chloride in the useless mercury catalyst.The present invention is by at high temperature leading to chlorine in mercurous solid waste, make Elemental Mercury or mercury salt in the mercurous solid waste be converted into mercury chloride, through high temperature carbonization mercury chloride is steamed again, form mercuric chloride solution with solvent absorbing gas phase chlorination mercury at last and can be directly used in the low solid mercury catalyst of production, gac after the destructive distillation is substantially residual without mercury chloride, still can be used for low solid mercury catalyst production or other side after modification.The whole process of the method produces without slag and effluent, and technique is simple, and is with low cost, simultaneously with the cyclic utilization of waste, has the advantage of environmental protection.
The recovery method of mercury in a kind of mercurous solid waste comprises being divided into step drying, chlorination, destructive distillation, the absorption operation of following order following steps and carrying out:
(1) drying: drying process is that mercurous solid waste is packed in the closed reactor, passes into the rare gas element drying under 100 ℃-200 ℃, and the time is 0.5-10 hour; Afterwards closed reactor is heated;
(2) chlorination: chlorination process is to the dry Cl that passes into to closed reactor after being preheated the device preheating under 200 ℃-400 ℃
2, rear persistently overheating, time of chlorinating 0.5-10 hour; Mercurous solid waste is fully contacted with chlorine, and the form of mercury becomes divalence mercury gradually;
(3) destructive distillation: retort process is to pass into rare gas element in closed reactor, and is warming up to 400 ℃-750 ℃ and carries out destructive distillation, and the destructive distillation time is 1-10 hour, and the mercurous solid waste after chloridized is carried out destructive distillation.
(4) absorb: absorption process is got rid of by closed reactor by the mercury chloride steam that destructive distillation goes out, the mercury chloride in the absorption gas phase that under dynamic action, circulate of the lyosorption in the circulating solvent storage tank, after deliver to circulation agent storage tank for standby use.
The present invention adopts drying, chlorination, destructive distillation, absorption step, reclaims mercury in the mercurous solid waste by above-mentioned steps, and organic efficiency is high, and easy and simple to handle, circulating solvent becomes mercuric chloride solution after absorbing mercury chloride, and for subsequent use after the removal of impurities after filtration, chloride tail gas is emptying after removing the evil.
The recovery method of mercury in described a kind of mercurous solid waste, the used rare gas element of drying process is one or more gas mixtures in nitrogen, helium, the argon gas.
The recovery method of mercury in described a kind of mercurous solid waste, closed reactor arrange heat conductive oil inlet and thermal oil outlet, and type of heating is heat-conducting oil heating, electrically heated or fuel direct heating.
The recovery method of mercury in described a kind of mercurous solid waste, the solvent that absorption process absorbs the mercury chloride in the gas phase is one or more the mixture in water, hydrochloric acid, nitric acid, chloroazotic acid, the hypochlorous acid, adopts the solvent of solubilized mercury chloride that the gas phase chlorination mercury that destructive distillation goes out is absorbed.
Mercurous solid waste of the present invention drying, chlorination, destructive distillation operation general mercury wherein in closed reactor are converted into mercury chloride and distill out, after absorbing, the circulating solvent that the mercury chloride steam comes via the circulating solvent pump delivery enters the circulating solvent storage tank, be delivered to storage tank for standby use by transferpump after solvent absorbing to be recycled is saturated, continue circulation by solvent makeup pump supplementing solvent after conveying is finished.
The invention provides a kind of method that reclaims mercury in the mercurous solid waste, be specially adapted to the recovery of mercury in the useless mercury catalyst of acetylene hydrochlorination.Mercury in the mercury-containing wastes exists mainly with the form of mercury chloride, subchloride of mercury, red precipitate, zunsober or mercury simple substance greatly, and experiment shows that the mercury of above-mentioned form at high temperature can lead to chlorine it is carried out chlorination generation mercury chloride.The method that the present invention carries arch is that mercurous solid waste is at high temperature led to chlorinated with chlorine, make mercury element wherein change into mercury chloride, then at high temperature logical nitrogen carries out destructive distillation, and the mercury chloride steam pumps into storage tank for standby use after solvent absorbing, or directly supplies with the production of low solid mercury catalyst; Simultaneously, the waste and old absorbent charcoal carrier after reclaiming still can be used for other industrial production after treatment, such as the production of low solid mercury catalyst and purification of the synthetic gas mixture of production of vinyl chloride by calcium carbide method etc.The present invention at first descends mercury-containing wastes dry 0.5-10 hour at 100 ℃-200 ℃, secondly 200 ℃-400 ℃ lower logical dry chlorine gas chlorinations 0.5-10 hour, then 400-750 ℃ of lower logical nitrogen destructive distillation 1-10 hour, use at last the solvent absorbing gas from dry distillation tail, mercury in the mercurous solid waste can be recycled with the form of mercury chloride, the mercury rate of recovery of the method can reach 80-99%.
The main chemical reactions equation of the method is:
Hg+Cl
2→HgCl
2+Q
1
Hg
2Cl
2+Cl
2→2HgCl
2+Q
2
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention 1.
Embodiment
Embodiment 1:
The recovery method of mercury in a kind of mercurous solid waste, comprise drying, chlorination, destructive distillation, absorption operation, be that 0.50% mercurous solid waste 2 is packed in the closed reactor 4 with the 500Kg mercury content, with closed reactor 2 heating, pass into thermal oil by heat conductive oil inlet 6, discharged by thermal oil outlet 3 after the heating, simultaneously logical N
2Drying, 150 ℃ of control temperature, 2 hours time of drying; Close N
2, pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2, after be warming up to 250 ℃ and continue 1 hour, be warming up to again 350 ℃ and continue 2 hours; Close Cl
2, in closed reactor, pass into N
2, be warming up to 450 ℃ and kept 2 hours, then be warming up to 550 ℃ and kept 3 hours; Pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2The time ON cycle solvent storage tank 5 power set, with the mercury chloride in the absorption by Hydrochloric Acid gas phase of 0.1mol/L, circulating solvent is for subsequent use after the removal of impurities after filtration, chloride tail gas is emptying after removing the evil.
Embodiment 2 is that with the difference of embodiment 1 absorption process can adopt spray equipment that the mercury chloride in the gas phase is absorbed.
The difference of embodiment 3 and embodiment 1 or 2 is to pass into a certain amount of dry Cl that is preheated after device 1 preheating in closed reactor
2, and keep certain pressure, and close closed reactor import and outlet, do not need the simultaneously power set of ON cycle solvent feed tank 5.
Embodiment 4
The recovery method of mercury in a kind of mercurous solid waste, comprise drying, chlorination, destructive distillation, absorption operation, be that 3.30% mercurous solid waste 2 is packed in the closed reactor 4 with the 500Kg mercury content, with closed reactor 2 heating, pass into thermal oil by heat conductive oil inlet 6, discharged by thermal oil outlet 3 after the heating, simultaneously logical N
2Drying, 200 ℃ of control temperature, 2 hours time of drying; Close N
2, pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2, after be warming up to 300 ℃ and continue 1.5 hours, be warming up to again 380 ℃ and continue 4 hours; Close Cl
2, in closed reactor, pass into N
2, be warming up to 480 ℃ and kept 3 hours, then be warming up to 650 ℃ and kept 5 hours; Pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2The time ON cycle solvent storage tank 5 power set, absorb mercury chloride in the gas phase with 80 ℃ hot deionized waters, circulating solvent is for subsequent use after the removal of impurities after filtration, chloride tail gas is emptying after removing the evil.
Embodiment 5
The recovery method of mercury in a kind of mercurous solid waste, comprise drying, chlorination, destructive distillation, absorption operation, be that 4.71% mercurous solid waste 2 is packed in the closed reactor 4 with the 500Kg mercury content, with closed reactor 2 heating, pass into thermal oil by heat conductive oil inlet 6, discharged by thermal oil outlet 3 after the heating, simultaneously logical N
2Drying, 200 ℃ of control temperature, 3 hours time of drying; Close N
2, pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2, after be warming up to 300 ℃ and continue 2 hours, be warming up to again 350 ℃ and continue 8 hours; Close Cl
2, in closed reactor, pass into N
2, be warming up to 450 ℃ and kept 3 hours, then be warming up to 750 ℃ and kept 6 hours; Pass into the dry Cl that is preheated after device 1 preheating in the good mercurous solid waste 3 of above-mentioned drying
2The time ON cycle solvent storage tank 5 power set, the HNO with 5%
3Absorb the mercury chloride in the gas phase, circulating solvent is for subsequent use after the removal of impurities after filtration, and chloride tail gas is emptying after removing the evil.
Claims (4)
1. the recovery method of mercury in the mercurous solid waste, comprise the step of following order: drying, chlorination, destructive distillation, absorption operation is characterized in that:
(1) drying: drying process is that mercurous solid waste is packed in the closed reactor, passes into the rare gas element drying under 100 ℃-200 ℃, and the time is 0.5-10 hour;
(2) chlorination: chlorination process is the dry chlorine gas that passes into to closed reactor after being preheated the device preheating under 200 ℃-400 ℃, rear persistently overheating, time of chlorinating 0.5-10 hour;
(3) destructive distillation: retort process is to pass into rare gas element in closed reactor, and is warming up to 400 ℃-750 ℃ and carries out destructive distillation, and the destructive distillation time is 1-10 hour;
(4) absorb: absorption process is discharged by closed reactor by the gas phase chlorination mercury that destructive distillation goes out, the mercury chloride in the absorption gas phase that under dynamic action, circulate of the lyosorption in the circulating solvent storage tank, after deliver to circulation agent storage tank for standby use.
2. the recovery method of mercury in a kind of mercurous solid waste as claimed in claim 1 is characterized in that the used rare gas element of drying process is one or more gas mixtures in nitrogen, helium, the argon gas.
3. the recovery method of mercury in a kind of mercurous solid waste as claimed in claim 1 is characterized in that closed reactor arranges heat conductive oil inlet and thermal oil outlet, and type of heating is heat-conducting oil heating, electrically heated or fuel direct heating.
4. the recovery method of mercury in a kind of mercurous solid waste as claimed in claim 1 is characterized in that solvent that absorption process absorbs the mercury chloride in the gas phase is one or more the mixture in water, hydrochloric acid, nitric acid, chloroazotic acid, the hypochlorous acid.
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| CN2012104674818A CN102942211A (en) | 2012-11-19 | 2012-11-19 | Method for recycling mercury from mercury-containing solid wastes |
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| CN2012104674818A CN102942211A (en) | 2012-11-19 | 2012-11-19 | Method for recycling mercury from mercury-containing solid wastes |
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Cited By (7)
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| CN103550989A (en) * | 2013-10-16 | 2014-02-05 | 贵州大龙银星汞业有限责任公司 | Comprehensive treatment method of tail gas in mercury chloride production process |
| CN104138706A (en) * | 2013-05-07 | 2014-11-12 | 贵州省万山银河化工有限责任公司 | Method using hydrochloric acid for resource recovery from tail gas of mercuric chloride production |
| CN104438285A (en) * | 2014-11-06 | 2015-03-25 | 中国科学院生态环境研究中心 | Method for carrying out innocent treatment on waste mercury catalyst by mechanical ball milling via taking sulfur as additive |
| CN104451204A (en) * | 2013-09-25 | 2015-03-25 | 新疆天业（集团）有限公司 | Mercury recovering and dry distillation device for waste mercury catalyst |
| CN107880970A (en) * | 2017-11-14 | 2018-04-06 | 华北电力大学（保定） | A kind of microwave radiation formula low-temperature pyrolysis of coal demercuration system and application method |
| CN108624756A (en) * | 2018-04-28 | 2018-10-09 | 张良儒 | A kind of recovery process of the useless mercury catalyst of low-consumption high-efficiency |
| CN112251607A (en) * | 2020-10-29 | 2021-01-22 | 新晃鲁湘钡业有限公司 | Processing method of mercury-containing waste |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104138706A (en) * | 2013-05-07 | 2014-11-12 | 贵州省万山银河化工有限责任公司 | Method using hydrochloric acid for resource recovery from tail gas of mercuric chloride production |
| CN104138706B (en) * | 2013-05-07 | 2016-12-28 | 贵州省万山银河化工有限责任公司 | A kind of HCl recovery mercuric chloride produces the method for tail gas |
| CN104451204A (en) * | 2013-09-25 | 2015-03-25 | 新疆天业（集团）有限公司 | Mercury recovering and dry distillation device for waste mercury catalyst |
| CN104451204B (en) * | 2013-09-25 | 2016-06-08 | 新疆天业（集团）有限公司 | A kind of useless mercury catalyst hydrargyrum reclaims destructive distillation device |
| CN103550989A (en) * | 2013-10-16 | 2014-02-05 | 贵州大龙银星汞业有限责任公司 | Comprehensive treatment method of tail gas in mercury chloride production process |
| CN103550989B (en) * | 2013-10-16 | 2015-10-28 | 贵州大龙银星汞业有限责任公司 | The integrated conduct method of tail gas in a kind of mercury chloride production process |
| CN104438285A (en) * | 2014-11-06 | 2015-03-25 | 中国科学院生态环境研究中心 | Method for carrying out innocent treatment on waste mercury catalyst by mechanical ball milling via taking sulfur as additive |
| CN104438285B (en) * | 2014-11-06 | 2019-12-24 | 中国科学院生态环境研究中心 | Method for innocent treatment of waste mercury catalyst by mechanical ball milling with sulfur as additive |
| CN107880970A (en) * | 2017-11-14 | 2018-04-06 | 华北电力大学（保定） | A kind of microwave radiation formula low-temperature pyrolysis of coal demercuration system and application method |
| CN107880970B (en) * | 2017-11-14 | 2023-10-31 | 华北电力大学（保定） | Microwave radiation type coal low-temperature pyrolysis mercury removal system and use method thereof |
| CN108624756A (en) * | 2018-04-28 | 2018-10-09 | 张良儒 | A kind of recovery process of the useless mercury catalyst of low-consumption high-efficiency |
| CN112251607A (en) * | 2020-10-29 | 2021-01-22 | 新晃鲁湘钡业有限公司 | Processing method of mercury-containing waste |
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Application publication date: 20130227 |