CN103991924B - A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater - Google Patents
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater Download PDFInfo
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Abstract
The invention discloses a kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, the sodium sulfate of employing concentration 5 ~ 6% or sulphuric acid soln are as regenerated liquid, 001*7 gel-network precipitation method after to be 5 ~ 6BV/h saturated to absorption with flow by regenerated liquid carries out desorption and regeneration, when regenerated liquid volume reaches 4 ~ 5 times of resin bed effective volume, regeneration completes.The invention has the beneficial effects as follows: using regenerated liquid volumetric usage as indicating the signal regenerated, can realize quick automatic switching regeneration and adsorption process in engineer applied.This renovation process regeneration efficiency reaches 90 ~ 95%, higher than conventional regeneration mode.The present invention adopts single kind regenerated liquid, reduces regenerated liquid usage quantity.Regeneration system rapidly device is single, reduces one-time investment cost; Regeneration solution concentration is low, and reagent cost is low.Non-regenerative operating procedure is simple, easily realizes Automated condtrol; Renovation process can operate flexibly.
Description
Technical field
The present invention relates to a kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater.
Background technology
Electrolytic manganese is the second largest industry in China's ferrous metallurgy field, and highly purified manganese metal is all obtained by wet method electrolysis.China sets up Article 1 electrolytic manganese production line so far from nineteen fifty-three in Shanghai, through the development of over half a century, and existing nearly 200 the electrolytic manganese enterprises in the whole nation at present.In recent years due to the demand that Gao Mengdi town austenite 200 is Stainless Steel extensive development, electrolytic manganese industry is pushed to a larger market.In addition, 400 of Fe-Mn-N system is that the research work of Stainless Steel is also deeply being carried out, and what its partial properties exceeded based on Cr 300 is Stainless Steel, and the development for electrolytic manganese industry is brought more wide space again by this.
From geographical position, electrolytic manganese enterprise of China many places are in remote mountain area, and great majority are territories, ethnic minority live inconcentrated communities, local economic development falls behind, manganese ore exploitation and processing are its mainstay industries, at the local a large amount of Employment of solution, increase local resident's income, safeguard and play irreplaceable effect in regional stability and national unity etc.With regard to " manganese triangle " area, 2008, the Xiushan Mn-industry gross output value accounted for more than 80% of whole county gross industrial output value, and manganese industry provides tax revenue to account for 50% of whole county fiscal revenue, provided job more than 10,000; Huayuan, Hunan manganese industry tax revenue accounts for 46% of whole county fiscal revenue, provides job more than 10,000; The Guizhou Province Song Taoxian manganese industry output value accounts for 80% of whole county gross industrial output value, provides job more than 6000.
Electrolytic manganese industry, while making major contribution for local economic construction, causes serious environmental pollution.The problem of environmental pollution of the sector mainly comprises water pollutions, industrial residue pollution and topsoil, such as: chemical combination press filtration workshop section ground and filter cloth washing, the cleaning of potroom pole plate and ground flushing, useless passivating solution, slag field water from diffusion etc. cause a large amount of trade effluents containing high density heavy metal produced; The Industrial Solid Wastes such as the waste residue that chemical combination liquid, processing wastewater process produce and the anode sludge that electrolytic process produces; The waste gas such as the dust that pulverizing, product stripping etc. produce and chemical combination, electrolytic process generation ammonia mist, acid mist.Wherein, waste water pollution problem is one of key issue of restriction electrolytic manganese industry value chain.The very high concentrations of vitriol, ammonia nitrogen, manganese in waste water, the concentration of chromium, selenium is also higher, under prior art condition, vitriol, ammonia nitrogen, Meng Deng contamination index usually can not stably reaching standards in waste water after treatment, cause severe contamination to the surface water of surrounding, underground water, bed mud in river, soil.
" manganese triangle " event in 2005, causes the great attention of relevant department of State Council to electrolytic manganese, policy advance to perfect order such as " manganese triangle " local pollution control comprehensive improvement and electrolytic manganese industry access etc.Electrolytic manganese industry overall technology level increased in recent years; environmental protection work is strengthened to some extent; the situation of electrolytic manganese enterprise has more several years ago had very large change; but electrolytic manganese production process is still very serious to the problem of environmental pollution caused, and its resource consumption and gross contamination emission are still in higher level.
Environmental pollution oneself become the significant problem faced in China's current development, the old road that China never can walk " first polluting, rear improvement ", the working dynamics that effective measure strengthens environment protection must be got by Bian.Cleaner production is a kind of new model of development of modern industry; it is advocated decontamination as far as possible, reduces environmental hazard and resource rational utilization, slows down Resource exhaustion; also can be summarized as seek bottom line produce pollute and ceiling utilize resource; its core is that to replace the cleaner production of " end " Control pollution strategy with " whole process " Control pollution strategy be realize environment protection strategy to be turned to by end-of-pipe control and pollute the only way of Whole Process Control; also implement a scientific outlook on development, guide the important channel that enterprise takes a new road to industrialization.Electrolytic manganese industry as " three high and one low " industry of typical high investment, high energy consumption, high pollution, poor benefit, carry out energetically and implement the Green Sustainable of cleaner production to industry have have to be important meaning.
Summary of the invention
The object of the invention is to the shortcoming overcoming prior art, a kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater is provided.
Object of the present invention is achieved through the following technical solutions: a kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, the sodium sulfate of employing concentration 5 ~ 6% or sulphuric acid soln are as regenerated liquid, 001*7 gel-network precipitation method after to be 5 ~ 6BV/h saturated to absorption with flow by regenerated liquid carries out desorption and regeneration, when regenerated liquid volume reaches 4 ~ 5 times of resin bed effective volume, regeneration completes.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid.
The present invention has the following advantages: regenerated liquid flow of the present invention does not need priority control, and when regenerated liquid volume reaches 4 ~ 5 times of resin bed effective volume, regeneration completes.Like this, using regenerated liquid volumetric usage as indicating the signal regenerated, quick automatic switching regeneration and adsorption process can be realized in engineer applied.This renovation process regeneration efficiency reaches 90 ~ 95%, higher than conventional regeneration mode.The present invention adopts single kind regenerated liquid to regenerate, and can greatly reduce regenerated liquid usage quantity.Regeneration system rapidly device is single, reduces one-time investment cost; Regeneration solution concentration is low, and regenerative agent usage quantity is less, and reagent cost is low, and follow-up operation maintenance cost is few.Non-regenerative operating procedure is simple, easily realizes Automated condtrol.This renovation process can operate flexibly, both can unsteady flow speed run, can also high-speed cruising, can judge whether regeneration completes, and can realize quick automatic switching working order by controlling regenerated liquid consumption.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and protection scope of the present invention is not limited to the following stated:
embodiment 1:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sodium sulfate of concentration 5% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 6BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 3 times of absorption feed liquor flow, when regenerated liquid volume reaches 4 times of resin bed effective volume, regeneration completes, and the recovery time is 2.5h.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
embodiment 2:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sodium sulfate of concentration 5.5% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 5BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 2 times of absorption feed liquor flow, when regenerated liquid volume reaches 5 times of resin bed effective volume, the recovery time is 3.5h, and regeneration completes.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
embodiment 3:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sodium sulfate of concentration 6% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 5.5BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 1.7 times of absorption feed liquor flow, when regenerated liquid volume reaches 4.5 times of resin bed effective volume, the recovery time is 3h, and regeneration completes.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
embodiment 4:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sulphuric acid soln of concentration 5% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 6BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 3 times of absorption feed liquor flow, when regenerated liquid volume reaches 4 times of resin bed effective volume, regeneration completes, and the recovery time is 2.5h.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
embodiment 5:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sulphuric acid soln of concentration 5.5% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 5BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 2 times of absorption feed liquor flow, when regenerated liquid volume reaches 5 times of resin bed effective volume, the recovery time is 3.5h, and regeneration completes.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process
embodiment 6:
A kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, adopt the sulphuric acid soln of concentration 6% as regenerated liquid, be reversed with feed liquor direction during absorption, 001*7 gel-network precipitation method after to be 5.5BV/h with flow by regenerated liquid saturated to absorption carries out desorption and regeneration, feed liquor flow is 1.7 times of absorption feed liquor flow, when regenerated liquid volume reaches 4.5 times of resin bed effective volume, the recovery time is 3h, and regeneration completes.
The material such as sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
The step of employing 001*7 gel-network precipitation method process electrolytic manganese production technique tail end wastewater is:
S1, resin pre-treatment: with 10 ~ 15% concentration Na of 1.5 ~ 2.5 times of resin volumes
2sO
4solution or 20 ~ 25% concentration H
2sO
4solution soaking 001*7 gel-network precipitation method 6 ~ 10h, 2 ~ 6% concentration HCl solution of 1.5 ~ 2.5 times of resin volumes are adopted to carry out immersion 001*7 gel-network precipitation method 3 ~ 5h after cleaning, then clean water is to neutral, then adopts 2 ~ 6% concentration NaOH solution of 1.5 ~ 2.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 3 ~ 5h;
S2, absorption: resin absorption process adopts counter current absorption mode to carry out, namely feed liquor mode is for carry out from the bottom up, comparatively slowly balanced rising liquid level can be formed, ensure that Electrolytic Manganese Wastewater fully can contact with 001*7 gel-network precipitation method layer pretreated in step S1, the micro-filtration that waste water is promoted to Di front end through lift pump is filtered, remove fine impurity particle, prevent from blocking resin layer, reflux type enters resin bed body subsequently, standard water discharge discharge after treatment.In adsorption process, 001*7 resin Preferential adsorption mn ion, then the ammonia nitrogen ion in waste water is adsorbed, and displace the original sodium ion (or hydrogen ion) carried of ion exchange resin, the feed liquor flow of Electrolytic Manganese Wastewater is 2 ~ 3BV/h, and resin absorption capacity is 0.28(mol ammonia nitrogen)/(L wet resin).
And then the resin after utilizing renovation process of the present invention saturated to absorption carries out desorption and regeneration.
Current resin universal preprocessing method is:
(1) salt solution process: with general 2 times of resin volumes, the common salt aqueous solution of 10% soaks more than 20 hours, then puts salt solution, with tap water to pH is neutrality.
(2) dilute hydrochloric acid process: with general 2 times of resin volumes, the hydrochloric acid of 2% ~ 5% concentration, soak after 4 ~ 8 hours, more repeatedly rinse to pH is neutrality with tap water.
(3) diluted sodium hydroxide solution process: by general 2 times of resin volumes, the oxygen sodium hydroxide solution of 2% ~ 5% concentration, soak after 4 ~ 8 hours, more repeatedly rinse to pH is neutrality with tap water.
This pretreatment process is resin universal preprocessing method, be applicable to the wastewater treatment of the Single Pollution material of lower concentration, but high for this Pollutant levels of Electrolytic Manganese Wastewater, the waste water that pollutant kind is numerous and diverse, resin can not thoroughly excite by original pretreatment process, makes it to reach best effect.Original pretreatment process amount of consumption of drugs is comparatively large, and operating process is complicated.
And pre-treatment resin object of the present invention is 001*7 strong acidic ion resin, namely the pre-treatment the first step skips the pretreated mode of conventional resins, direct employing high density regenerated liquid, i.e. 20% concentration acid (or 10% sodium sulfate) process, resin is made directly to adopt regenerated liquid to excite, the foreign ion etc. adsorbed in resin is made full use of the impellent of concentration difference, desorb goes out foreign ion, pretreated resin is made to have larger specific surface area and porosity, improve adsorptive power and desorption efficiency, in use can work under the condition of high concentrated acid; The present invention only needs a procedure to carry out resin pre-treatment, reduces oxygen-consumption, saves pre-treatment cost.
In prior art, the general renovation process of resin adopts sodium-chlor and hydrochloric acid as regeneration, and first adopting the NaCl solution of 8 ~ 10% just to wash, is 1.5 ~ 2 with resin volume ratio, and feed liquor flow velocity is 5 ~ 8m/h, recovery time >60min; Adopting 4 ~ 5%HCl solution to carry out backwash subsequently, is 2 ~ 3 with resin volume ratio, and feed liquor flow velocity is 5 ~ 8m/h, recovery time >60min.The method regeneration efficiency is 70 ~ 80%.
Original regeneration, can introduce chlorion during regeneration, regeneration product has the materials such as ammonium chloride, if direct reuse, can bring a large amount of chlorion into, cause production process to affect.Regenerative process is complicated, needs to regenerate with two kinds of regenerated liquids; Regenerated liquid consumption is large, and causing regeneration waste liquid to recycle difficulty increases greatly.
Regenerated liquid flow of the present invention does not need priority control, and when regenerated liquid volume reaches 4 ~ 5 times of resin bed effective volume, regeneration completes.Like this, using regenerated liquid volumetric usage as indicating the signal regenerated, quick automatic switching regeneration and adsorption process can be realized in engineer applied.This renovation process regeneration efficiency reaches 90 ~ 95%.The present invention adopts single kind regenerated liquid to regenerate, and can greatly reduce regenerated liquid usage quantity.Regeneration system rapidly device is single, reduces one-time investment cost; Regeneration solution concentration is low, and regenerative agent usage quantity is less, and reagent cost is low, and follow-up operation maintenance cost is few.Non-regenerative operating procedure is simple, easily realizes Automated condtrol.Regeneration efficiency reaches 90 ~ 95%, higher than conventional regeneration mode.This renovation process can operate flexibly, both can unsteady flow speed run, can also high-speed cruising, can judge whether regeneration completes, and can realize quick automatic switching working order by controlling regenerated liquid consumption.
In above-described embodiment, ammonia nitrogen influent concentration is 300mg/L, and consider the situation of its fluctuation change, the variation factor by 1.2 is considered, then designing influent concentration is 360mg/L; When aqueous concentration is greater than 15mg/L, namely exceed emission standard, then think that resin needs manipulation of regeneration.
Processing the water yield every day is 30t, amounts to TAN to be processed to be:
m=Q*(C
0-C
e)=30×（360-15）=10350g
Again, the exchange adsorption capacity of dynamic adsorption process 001x7 strong acidic ion resin is 0.28(mol ammonia nitrogen)/(L wet resin), therefore the resin humid volume amount processing 10350g ammonia nitrogen needs every day is:
10350 ÷ 18 ÷ 0.28=2053.6L, are 2.1m
3;
Consider that 5d is a regeneration period, then single ion exchange resin effective volume is 10.5m
3, size is: φ 2200*3800mm.
Consider the impact of waste water impurity, process design is: waste water---micro-filtration---ion exchange reaction device
Micro-filtration is designed to two cover parallel devices, a set of use, another set of cleaning; Ion-exchange absorption tank is two covers, and absorption, regeneration are used alternatingly.
Claims (2)
1. the regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater, it is characterized in that: adopt concentration be 5 ~ 6% sodium sulfate or concentration be that the sulphuric acid soln of 5 ~ 6% is as regenerated liquid, 001*7 gel-network precipitation method after to be 5 ~ 6BV/h saturated to absorption with flow by regenerated liquid carries out desorption and regeneration, when regenerated liquid volume reaches 4 ~ 5 times of Di effective volume, regeneration completes, and regenerated liquid becomes regeneration waste liquid;
The step of 001*7 gel-network precipitation method process electrolytic manganese production technique tail end wastewater is adopted to comprise:
S1, resin pre-treatment: with 10 ~ 15% concentration Na of 1.5 ~ 2.5 times of resin volumes
2sO
4solution or 20 ~ 25% concentration H
2sO
4solution soaking 001*7 gel-network precipitation method 6 ~ 10h, 2 ~ 6% concentration HCl solution of 1.5 ~ 2.5 times of resin volumes are adopted to carry out immersion 001*7 gel-network precipitation method 3 ~ 5h after cleaning, then clean water is to neutral, then adopts 2 ~ 6% concentration NaOH solution of 1.5 ~ 2.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 3 ~ 5h;
S2, absorption: resin absorption process adopts counter current absorption mode to carry out, namely feed liquor mode is for carry out from the bottom up, comparatively slowly balanced rising liquid level can be formed, ensure that electrolytic manganese production technique tail end wastewater fully can contact with 001*7 gel-network precipitation method layer pretreated in step S1, the micro-filtration that waste water is promoted to Di front end through lift pump is filtered, remove fine impurity particle, prevent from blocking resin layer, reflux type enters Di subsequently, standard water discharge discharge after treatment; In adsorption process, 001*7 gel-network precipitation method Preferential adsorption mn ion, then the ammonia nitrogen ion in waste water is adsorbed, and displace the original sodium ion that carries of 001*7 ion exchange resin or hydrogen ion, the feed liquor flow of electrolytic manganese production technique tail end wastewater is 2 ~ 3BV/h, and resin absorption capacity is 0.28(mol ammonia nitrogen)/(L wet resin).
2. a kind of regeneration of ion-exchange resin method for the treatment of electrolytic manganese production technique tail end wastewater according to claim 1, it is characterized in that: sulfur acid manganese, ammonium sulfate in described regeneration waste liquid, first 1 hour regenerated liquid direct reuse of resin regeneration is in electrolytic manganese production process, wherein ammonia nitrogen concentration content is greater than 4g/L, the regenerated liquid of resin regeneration after 1 hour carries out cyclic regeneration, namely regenerated liquid regenerate after regeneration waste liquid water outlet directly get back in the hold-up vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid.
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| CN105080624B (en) * | 2015-09-10 | 2018-04-10 | 舒城联科环境科技有限公司 | A kind of ion exchange resin regeneration method |
| CN105293584B (en) * | 2015-10-21 | 2017-10-20 | 广西银亿再生资源有限公司 | A kind of method of purification of sulphuric acids manganese solution |
| CN105695751B (en) * | 2016-03-11 | 2017-08-25 | 武汉工程大学 | A kind of purification technique of electrolytic manganese anode mud |
| CN109569745A (en) * | 2018-12-06 | 2019-04-05 | 中电环保股份有限公司 | Cation exchange resin automatic regeneration device and method |
| CN110624611A (en) * | 2019-03-27 | 2019-12-31 | 兆德（南通）电子科技有限公司 | Cation resin regeneration process |
| CN114163685A (en) * | 2020-09-10 | 2022-03-11 | 阳江核电有限公司 | Waste resin regeneration treatment method |
| CN114272961B (en) * | 2021-12-20 | 2023-10-03 | 江西永兴特钢新能源科技有限公司 | Ion exchange resin regeneration method for removing impurities from lithium sulfate solution |
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