CN103990499B - A kind of preprocess method of the ion exchange resin for the treatment of electrolytic manganese production technique tail end wastewater - Google Patents
A kind of preprocess method of the ion exchange resin for the treatment of electrolytic manganese production technique tail end wastewater Download PDFInfo
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- CN103990499B CN103990499B CN201410248839.7A CN201410248839A CN103990499B CN 103990499 B CN103990499 B CN 103990499B CN 201410248839 A CN201410248839 A CN 201410248839A CN 103990499 B CN103990499 B CN 103990499B
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Abstract
The invention discloses a kind of preprocess method of the ion exchange resin for the treatment of electrolytic manganese production technique tail end wastewater, with 10 ~ 15% concentration Na of 1.5 ~ 2.5 times of resin volumes
2sO
4or 20 ~ 25% concentration H
2sO
4solution soaks 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 soak 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 3 ~ 5h.The invention has the beneficial effects as follows: make pretreated resin have larger specific surface area and porosity, improve adsorption capacity 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 pretreatment, reduces oxygen demand, saves pretreatment cost.
Description
Technical field
The present invention relates to a kind of preprocess method of the ion exchange resin for the treatment of electrolytic manganese production technique tail end wastewater.
Background technology
Electrolytic manganese is the second largest industry in China's iron and steel industry 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 pillar 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 total industrial output value, and manganese industry provides tax revenue to account for 50% of whole county fiscal revenues, provided job more than 10,000; Huayuan, Hunan manganese industry tax revenue accounts for 46% of whole county fiscal revenues, provides job more than 10,000; The Guizhou Province Song Taoxian manganese industry output value accounts for 80% of whole county total 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 atmosphere pollution, 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 leakage water etc. cause a large amount of industrial wastewaters containing high concentration heavy metal produced; The Industrial Solid Wastes such as the waste residue that chemical combination liquid, technique waste water process produce and the earth of positive pole 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 sulfate, ammonia nitrogen, manganese in waste water, the concentration of chromium, selenium is also higher, under prior art condition, sulfate, 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 environmental protection must be got by Bian.Cleaner production is a kind of new model of development of modern industry; it is advocated pollution abatement 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 maximum 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 preprocess method of the ion exchange resin 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 preprocess method of the ion exchange resin for the treatment of electrolytic manganese production technique tail end wastewater, with 10 ~ 15% concentration Na of 1.5 ~ 2.5 times of resin volumes
2sO
4solution or 20 ~ 25% concentration H
2sO
4solution soaks 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 soak 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.
The present invention has the following advantages: namely the pretreatment first step of the present invention skips the pretreated mode of conventional resins, direct employing high concentration regenerated liquid, i.e. 20% concentration acid (or 10% sodium sulphate) process, resin is made directly to adopt regenerated liquid to excite, the foreign ion etc. adsorbed in resin is made full use of the motive force of concentration difference, desorb goes out foreign ion, pretreated resin is made to have larger specific surface area and porosity, improve adsorption capacity 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 pretreatment, reduces oxygen demand, saves pretreatment cost.
The present invention has optimized the ion exchange resin being suitable for processing ammonia nitrogen in electrolytic manganese industry waste water, and the anti-manganese ion interference performance of this ion exchange resin is large, and after regeneration, heavy adsorption capacity is effective, and cost is low, and cost performance is high.
Detailed description of the invention
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:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 15% concentration Na of 1.5 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 6h, 6% concentration HCl solution of 1.5 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 3h after cleaning, then clean water is to neutral, then adopts 2% concentration NaOH solution of 2.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 5h.
embodiment 2:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 12% concentration Na of 2 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 8h, 4% concentration HCl solution of 2 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 4h after cleaning, then clean water is to neutral, then adopts 4% concentration NaOH solution of 2 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 4h.
embodiment 3:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 10% concentration Na of 2.5 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 10h, 2% concentration HCl solution of 2.5 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 5h after cleaning, then clean water is to neutral, then adopts 2% concentration NaOH solution of 1.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 3h.
embodiment 4:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 25% concentration H of 1.5 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 6h, 6% concentration HCl solution of 1.5 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 3h after cleaning, then clean water is to neutral, then adopts 2% concentration NaOH solution of 2.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 5h.
embodiment 5:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 22% concentration H of 2 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 8h, 4% concentration HCl solution of 2 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 4h after cleaning, then clean water is to neutral, then adopts 4% concentration NaOH solution of 2 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 4h.
embodiment 6:
For the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, with 20% concentration H of 2.5 times of resin volumes
2sO
4solution soaks 001*7 gel-network precipitation method 10h, 2% concentration HCl solution of 2.5 times of resin volumes is adopted to carry out immersion 001*7 gel-network precipitation method 5h after cleaning, then clean water is to neutral, then adopts 2% concentration NaOH solution of 1.5 times of resin volumes to carry out immersion 001*7 gel-network precipitation method 3h.
The method of above-mentioned pretreated 001*7 gel-network precipitation method process electrolytic manganese production technique tail end wastewater comprises the following steps:
Absorption: resin adsorption 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 elevator pump is filtered, remove fine impurity particle, prevent from blocking resin bed, reflux type enters resin bed body subsequently, standard water discharge discharge after treatment.In adsorption process, 001*7 resin Preferential adsorption manganese 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 adsorption capacity is 0.28(mol ammonia nitrogen)/(L wet resin);
Resin regeneration: the sodium sulphate of employing concentration 5 ~ 6% or sulfuric acid solution are as regenerated liquid, be reversed with feed liquor direction during absorption, resin after to be 5 ~ 6BV/h saturated to absorption with flow by regenerated liquid carries out desorption and regeneration, recovery time is 2.5 ~ 3.5h, feed liquor flow is 1 ~ 3 times of absorption feed liquor flow, 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 regeneration liquid waste, 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 circular regeneration, namely regenerated liquid regenerate after regeneration liquid waste water outlet directly get back in the holding vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
Current resin universal preprocessing method is:
(1) saline solution process: with general 2 times of resin volumes, the common salt aqueous solution of 10% soaks more than 20 hours, then puts saline solution, with tap water to pH is neutrality.
(2) watery 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 running 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 running water.
This preprocess method is resin universal preprocessing method, be applicable to the wastewater treatment of the Single Pollution material of low 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 preprocess method, makes it to reach optimum efficiency.Original preprocess method amount of consumption of drugs is comparatively large, and operating process is complicated.
And pretreatment resin object of the present invention is 001*7 strong acidic ion resin, namely the pretreatment first step skips the pretreated mode of conventional resins, direct employing high concentration regenerated liquid, i.e. 20% concentration acid (or 10% sodium sulphate) process, resin is made directly to adopt regenerated liquid to excite, the foreign ion etc. adsorbed in resin is made full use of the motive force of concentration difference, desorb goes out foreign ion, pretreated resin is made to have larger specific surface area and porosity, improve adsorption capacity 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 pretreatment, reduces oxygen demand, saves pretreatment cost.
In prior art, the general renovation process of resin adopts sodium chloride 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 liquid waste 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 use amount.Regenerative system device is single, reduces one-time investment cost; Regeneration solution concentration is low, and regenerative agent use amount 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 duty 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 coefficient by 1.2 is considered, then designing influent concentration is 360mg/L; When aqueous concentration is greater than 15mg/L, namely exceed discharge standard, then think that resin needs regeneration process.
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, design size is: φ 2200*3800mm.
Consider the impact of waste water impurity, technical flow design is: waste water---micro-filtration---ion-exchange reactions 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 (1)
1. for the treatment of a preprocess method for the ion exchange resin of electrolytic manganese production technique tail end wastewater, it is characterized in that: with 10 ~ 15% concentration Na of 1.5 ~ 2.5 times of resin volumes
2sO
4solution or 20 ~ 25% concentration H
2sO
4solution soaks 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 soak 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;
The method of pretreated 001*7 gel-network precipitation method process electrolytic manganese production technique tail end wastewater is adopted to comprise the following steps:
Absorption: resin adsorption 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 above-mentioned pretreated 001*7 gel-network precipitation method layer, the micro-filtration that waste water is promoted to Di front end through elevator pump is filtered, and removes fine impurity particle, prevents from blocking resin bed, reflux type enters resin bed body subsequently, standard water discharge discharge after treatment; In adsorption process, 001*7 resin Preferential adsorption manganese ion, adsorbs the ammonia nitrogen ion in waste water then, and displaces the original sodium ion that carries of ion exchange resin or hydrogen ion, the feed liquor flow of Electrolytic Manganese Wastewater is 2 ~ 3BV/h, and resin adsorption capacity is 0.28(mol ammonia nitrogen)/(L wet resin);
Resin regeneration: the sodium sulphate of employing concentration 5 ~ 6% or sulfuric acid solution are as regenerated liquid, be reversed with feed liquor direction during absorption, resin after to be 5 ~ 6BV/h saturated to absorption with flow by regenerated liquid carries out desorption and regeneration, recovery time is 2.5 ~ 3.5h, feed liquor flow is 1 ~ 3 times of absorption feed liquor flow, when regenerated liquid volume reaches 4 ~ 5 times of resin bed effective volume, regeneration completes; Sulfur acid manganese, ammonium sulfate material in regeneration liquid waste, 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 circular regeneration, namely regenerated liquid regenerate after regeneration liquid waste water outlet directly get back in the holding vessel of regenerated liquid, the regenerated liquid of this volume uses as next batch recovering liquid, is the equal of one and recycles process.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838064A (en) * | 2010-01-26 | 2010-09-22 | 中国环境科学研究院 | Method for recycling manganese ion in electrolytic manganese production tail end wastewater |
| CN102898306A (en) * | 2012-10-09 | 2013-01-30 | 常熟富士莱医药化工有限公司 | Synthetic method of monomethyl adipate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838064A (en) * | 2010-01-26 | 2010-09-22 | 中国环境科学研究院 | Method for recycling manganese ion in electrolytic manganese production tail end wastewater |
| CN102898306A (en) * | 2012-10-09 | 2013-01-30 | 常熟富士莱医药化工有限公司 | Synthetic method of monomethyl adipate |
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