CN1326622C - Process for reactivating gel type strong base negative resin of polluted in industrial water treatment - Google Patents
Process for reactivating gel type strong base negative resin of polluted in industrial water treatment Download PDFInfo
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- CN1326622C CN1326622C CNB2005100100335A CN200510010033A CN1326622C CN 1326622 C CN1326622 C CN 1326622C CN B2005100100335 A CNB2005100100335 A CN B2005100100335A CN 200510010033 A CN200510010033 A CN 200510010033A CN 1326622 C CN1326622 C CN 1326622C
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Abstract
The present invention provides a recovery method for polluted gel-type strong alkali yin resin in industrial water processing. The method comprises: step one, mechanical strength is detected; step two, the pollution type of polluted resin is identified; step three, recovery processing is orderly carried out according to the resin pollution type identified in step two and the order of oil pollution removal, iron pollution removal and organic pollution removal. A lower inlet of a polluted resin yin bed is connected with a metering pump, a white steel tank and a backwashing tank; an upper inlet of the backwashing tank is connected with an upper outlet of the polluted resin yin bed to form a recovery circulation system. The method of the present invention carries out recovery processing to polluted ion anion resin of a gel type and a strong base type in a production department under the condition of no influence on regular production. The present invention provides corresponding resin recovering methods according to different polluted conditions of the resin.
Description
(1) technical field
What the present invention relates to is a kind of ancillary technique of water treatment, reactivating gel type strong base negative resin of polluted technology in specifically a kind of Treatment of Industrial Water.
(2) background technology
Ion exchange resin is widely used in the water treatment technology of every field such as electric power, electronics, medicine, food, be used to produce various demineralized waters, pure water and ultra-pure water, and normal " strong acid type cationic resin-degassing-strong base resin anion (R.A.) " compound desalination process that adopts, be that pretreated water inlet is earlier through strong acid sun bed resin, remove cations such as calcium, magnesium, sodium, water outlet is an acid water, removes CO by the removing carbon dioxide device subsequently
2, remove anion such as sulfate radical, chlorion, bicarbonate radical, silicate in the water by cloudy bed at last.
For surface water, adopt the conventional treatment process of coagulation, precipitation, filtration, charcoal absorption usually.This technology is mainly removed suspension and the colloidal substance in the source water, with delivery turbidity, colourity and iron manganese content as control target, but it is lower to natural organic matter such as humic acid, fulvic acid and artificial synthetic various organic compound pollutants removal rates, so that after the experience preliminary treatment, still have a certain amount of chemical combination pollutant to enter cloudy bed, it is polluted.
After strong base negative resin is contaminated, progressively deepen from seeing color in appearance, exchange capacity descends, and the wash water amount increases, and going out water conductivity increases, and outlet water organic substance and dioxide-containing silica increase.The exchange capacity of resin descends, and the system water cycle shortens, and has increased the number of times of regeneration and the consumption of regenerative agent, and frequent regeneration also will influence the normal operation of production technology.In addition, desalted water is mainly supplied with the medium and high pressure boiler, produces the running of steam pushing turbine.Organic matter in the water enters the boiler after heat and is decomposed into carbonic acid, formic acid, acetate, propionic acid, and turbine blade and boiler material are caused corrosion.After silicon entered boiler, at the condition formation silicon dirt of high temperature, it is uneven and accidents caused that boiler is heated.
Along with the increase of industrial water source water pollutant kind and concentration, the situation that the common strong base negative resin that adopts is polluted in the Treatment of Industrial Water becomes increasingly complex, and conventional regeneration technology has been difficult to recover effectively the exchange capacity of resin.
(3) summary of the invention
The object of the present invention is to provide a kind of can the influence under the precondition of producing normal operation, recovery negative resin in short time, make the level of the approaching new resin of exchange capacity after negative resin is recovered, process for reactivating gel type strong base negative resin of polluted in the Treatment of Industrial Water of reduction regeneration alkaline consumption.
The object of the present invention is achieved like this:
The first step: detect mechanical strength
Detect the wear-resisting rate and the mill back rate of small round spheres of resin, select wear-resisting rate greater than 85%, mill back rate of small round spheres is greater than the processing of recovering of 75% resin;
Second step: the discriminating of the resin stain type of getting dirty
The resin that takes a morsel is put into test tube, and the water of the twice of reinjecting resin volume after vibration, determines that with AAS greasy dirt dyes degree;
The resin that takes a morsel is put into test tube, soaks resin 30 minutes with the 6mol/L concentrated hydrochloric acid, takes out a part of acid solution, to wherein dripping saturated potassium ferrocyanide, determines that resin is subjected to the iron pollution degree;
The resin that takes a morsel is put into test tube, sodium chloride solution immersion treatment with 10% 20-30 minute uses 10%NaCl and 4%NaOH mixed liquor 500ml again under 40 ℃ of conditions, soaks wet resin 24 hours, survey the total organic carbon (TOC) or the COD of soak, determine that resin is subjected to organic pollution level;
The 3rd step: pollute the resin recovery
According to the second resin stain type that identify of step, pollute, remove iron pollution, remove the order of organic contamination according to oil removing, select according to the processing of recovering successively of following a kind of or more than one methods:
1, the greasy dirt processing method of dying: resin is that 8% NaCl solution is regenerated with concentration earlier, under 40-50 ℃ of temperature, carry out oil removing as resuscitation fluid with 0.1%-0.2% non-ionic surface active agent FL-9 (polytrifluorochloroethylene), the cumulative volume of resuscitation fluid is 2 times of resin volume, pour out the recovery waste liquid after the processing, the resin after the recovery is clean with pure water rinsing.
2, the processing method of iron pollution: (1) with concentration be 10%, temperature is 40 ± 2 ℃ sodium chloride, and resin was carried out circular treatment 2 hours, the discharging waste liquid, again with desalted water clean 2 hours to water outlet near neutral; (2) with desalted water the negative resin bed is full of, in concentration is 10% hydrochloric acid, adds sodium sulfite, make concentration of sodium sulfite reach 5%, under 40 ± 2 ℃ of temperature, discharge waste liquid after resin circulated 4 hours, with desalted water clean 2 hours to water outlet near neutral.
3, the processing method of organic contamination resin:
The processing method of slight organic contamination: compound concentration is 4% sodium hydroxide solution and 10% sodium chloride solution equal-volume mixed liquor, and allocate 0.4%Tritonx-100 (non-ionic surface active agent therein into, claim polyoxyethylene uncle octyl phenol again) assistant medicament, form resuscitation fluid, under 40 ℃ condition with resuscitation fluid to resin circular treatment 8-12 hour.
Severe organic is polluted the processing method of resin: allocate effective chlorine density in the equal-volume mixed liquor of 4%NaOH and 10%NaCl into and be and allocate 1% hydrogen peroxide in 0.5% clorox or 4%NaOH and the 10%NaCl equal-volume mixed liquor into and form resuscitation fluid, with resuscitation fluid to the resin processing 4 hours of recovering that circulates.
The technological process that the circulation recovery is handled is: the lower inlet and the measuring pump of the cloudy bed of contaminated resin, white steel tank, recoil cleaning of evaporator are linked to each other, and the upper inlet of recoil cleaning of evaporator and the cloudy bed of contaminated resin upper outlet are connected to form the recovery circulatory system.
Method of the present invention under the situation that does not influence ordinary production to the processing of recovering of the contaminated gel type strong base type resin anion (R.A.) of workshop.The contaminated situation different according to resin proposes corresponding resin recovery way.Organic matter at the difficult recovery of resin anion (R.A.) pollutes, and proposes unique resuscitation technique.In saline and alkaline mixed liquor (4%NaOH and 10%NaCl), allocate effective chlorine density into and be 0.5% clorox or allocate 1% hydrogen peroxide into and form resuscitation fluid and have and remove the ability that organic matter pollutes resin efficiently, last short and recovery back resin water-yielding capacity near new resin at saline and alkaline mixed liquor (4%NaOH and 10%NaCl).
Increase along with industrial water source water pollutant kind and concentration, the situation that the common strong base negative resin that adopts is polluted in the Treatment of Industrial Water becomes increasingly complex, conventional regeneration technology has been difficult to recover effectively the exchange capacity of resin, and with serious pollution resin need adopt resuscitation technique to recover its exchange capacity.Consider and newly purchase resin price higher (about 2.5 ten thousand yuan/ton), contaminated resin is carried out the recovery of exchange capacity, use saving a large amount of controlling water fees as the resuscitation technique that adopts economical and efficient.Present technique is passed through years of researches, labor the pollution feature and the pollution type of contaminated strong base resin anion (R.A.), at the contaminated characteristics of contaminated resin, the contaminated resin method for resuscitation of high-efficiency and economic is proposed, and proposition does not influence the resuscitation technique of ordinary production, production application proof present technique economical and efficient, average 3100 yuan/ton of recovery negative resin.
(4) description of drawings
Accompanying drawing is a process flow diagram of the present invention.
(5) specific embodiments
For example the present invention is done more detailed description below in conjunction with accompanying drawing:
The lower inlet of the cloudy bed 1 of contaminated resin is linked to each other with the following outlet of measuring pump 4, white steel tank 3, recoil cleaning of evaporator 2, and the upper inlet of recoil cleaning of evaporator and the cloudy bed of contaminated resin upper outlet are connected to form the recovery circulatory system.
White steel tank bottom is provided with electric heater unit and temperature controller, is used to adjust the temperature of resuscitation fluid, and the cylinder of steel that is used for the resin backwash by the water treatment workshop is regulated the resuscitation fluid volume, and the cumulative volume of recovery solution is about 2 times of resin volume.Join resuscitation fluid in white steel tank, with measuring pump resuscitation fluid is squeezed into cloudy bed, circulation is got back to white steel tank through back wash tank, and heating recovers the temperature of resuscitation fluid in white steel tank.Recovery finishes, and is limpid to water outlet with the cloudy bed of desalted water flushing, regenerates with the amount of regular regeneration medicament twice, carries out the comparison of the old resin effluent index of new resin bed and recovery back.
The first step: detect mechanical strength
Detect the wear-resisting rate and the mill back rate of small round spheres of resin by petro chemical industry portion of People's Republic of China (PRC) ministerial standard (HG 2-886-76).When the wear-resisting rate of resin greater than 85%, mill back rate of small round spheres was greater than 75% o'clock, the resin mechanical strength satisfies instructions for use, promptly resin structure is intact, and the value of the contaminated resin of recovery is arranged.
Second step: the depollution order of the resin of getting dirty and the discriminating of pollution type
The normal contaminated type of negative resin is that greasy dirt dyes, iron pollution and organic matter pollute, and at first will differentiate the pollution type of resin.Combined pollution in this way, its depollution is oil removing, deironing and organic matter removal pollutant in proper order, single in this way pollution then selects for use following corresponding resuscitation technique to get final product.
Test tube is put in the resin taking-up on a small quantity, and the water of the twice of reinjecting resin volume is observed the water surface and " rainbow " whether occurred after the fierceness vibration, judge that tentatively greasy dirt dyes degree, determines that with AAS greasy dirt dyes degree again.
Resin taken out put into test tube on a small quantity, soaked resin 30 minutes, take out a part of acid solution, to wherein dripping saturated potassium ferrocyanide, when in various degree Prussian blue precipitation, can assert that resin is subjected to the iron pollution degree with the 6mol/L concentrated hydrochloric acid.
Test tube is put in the resin taking-up on a small quantity, sodium chloride solution with 10% is handled, the color of the vibration back observation salt solution tentatively section of declaring is subjected to organic pollution level, use 10%NaCl and 4%NaOH mixed liquor 500ml again under 40 ℃ of conditions, soaked wet resin 24 hours, survey the total organic carbon (TOC) or the COD of soak, assert that resin is subjected to organic pollution level.
The 3rd step: pollute the resin recovery
According to be that independent greasy dirt dyes, iron pollution or organic contamination, still following a kind of, two kinds or three kinds of methods are selected in two kinds among them or three kinds of composite pollutions, pollute, remove again iron pollution according to first oil removing, the processing of recovering successively of the order of removing organic contamination at last
The method for resuscitation that greasy dirt dyes: resin is regenerated with 8% NaCl solution earlier, removes the Ca in the resin
2+With a part of iron ion, prevent the Ca (OH) that in the process of oil removing, produces
2The deposit fouling resin.In the time of 40-50 ℃, use 0.1%-0.2% non-ionic surface active agent FL-9 (polytrifluorochloroethylene) as the resuscitation fluid oil removing earlier.The cumulative volume of resuscitation fluid is 2 times of resin volume.After handling through recovery after a while, pour out the recovery waste liquid, the resin after the recovery is clean with pure water rinsing.
The method for resuscitation of iron pollution: the first step, ion exchange resin conversion.Sodium chloride is added in the white steel tank, adds the concentration to 10% of water adjustment sodium chloride, keep 40 ± 2 ℃ of temperature, the 2 hours discharging waste liquids that circulate clean 2 hours to the approaching neutrality of water outlet with desalted water.Second step, deironing.With desalted water the moon bed is full of, then 33% hydrochloric acid is added in the white steel tank, add water in the groove and make concentration of hydrochloric acid reach 10%.In groove, add sodium sulfite, make its concentration reach 5%.Under 40 ± 2 ℃ of conditions, circulate and discharge waste liquid after 4 hours, clean 2 hours to the approaching neutrality of water outlet with desalted water.
The method for resuscitation of slight organic contamination resin: can adopt saline and alkaline mixed liquor recovery, the sodium hydroxide solution of preparation 4% and 10% sodium chloride solution equal-volume mixed liquor, and allocate 0.4%Tritonx-100 (non-ionic surface active agent therein into, claim polyoxyethylene uncle octyl phenol again) assistant medicament, form resuscitation fluid, under 40 ℃ condition recovery 8-12 hour, method for resuscitation was seen Fig. 1.
Severe organic is polluted the method for resuscitation of resin: can adopt the chemical oxidization method recovery, when iron pollution occurring earlier with 5% sodium sulfite solution deironing.Dispose the resuscitation fluid organic matter removal again, allocate effective chlorine density in the saline and alkaline mixed liquor (4%NaOH and 10%NaCl) into and be 0.5% clorox or saline and alkaline mixed liquor (4%NaOH and 10%NaCl) and allocate 1% hydrogen peroxide into and form resuscitation fluid, recover got final product in 4 hours.
Concrete recovery process is given an example: being subjected to organic matter and iron pollution negative resin to recover 15 tons is example, and the cumulative volume of recovery solution is about 2 times of resin volume, carries out deironing, back organic matter removal earlier.
Ion exchange resin conversion.6 ton 98% sodium chloride is added in the white steel tank, adds the concentration to 10% of water adjustment sodium chloride, keep 40 ± 2 ℃ of temperature, the 2 hours discharging waste liquids that circulate clean 2 hours to the approaching neutrality of water outlet with desalted water.
Deironing.With desalted water the moon bed is full of, then 8.5 ton 33% hydrochloric acid is added in the white steel tank, add water in the groove and make concentration of hydrochloric acid reach 10%.In groove, add sodium sulfite, make its concentration reach 5%.Under 40 ± 2 ℃ of conditions, circulate and discharge waste liquid after 4 hours, clean 2 hours to the approaching neutrality of water outlet with desalted water
The recovery organic contamination.4% NaOH is squeezed into cloudy bed is full of cloudy bed, 3 ton 98% sodium chloride is added in the white steel tank, add the 640kg clorox again, by adding the concentration that water makes sodium chloride in the groove is 10%, with the concentration of sodium hydroxide solution mixing clorox effective chlorine be 0.5%, be under 35 ± 2 ℃ the condition in temperature, circulation recovery 4 hours, discharging waste liquid.
Remove residual oxidant.30 ton 3% sodium sulfite solution is squeezed into cloudy bed cloudy bed is full of, keep after 2 hours the discharging waste liquid.
Put into operation.Above four the step finish after, regenerate with the amount of 2 times of regular regeneration agent, put into operation.
Claims (1)
1, process for reactivating gel type strong base negative resin of polluted in a kind of Treatment of Industrial Water,
The first step: detect mechanical strength
Detect the wear-resisting rate and the mill back rate of small round spheres of resin, select wear-resisting rate greater than 85%, mill back rate of small round spheres is greater than the processing of recovering of 75% resin;
Second step: the discriminating of the resin stain type of getting dirty
The resin that takes a morsel is put into test tube, and the water of the twice of reinjecting resin volume after vibration, determines that with AAS greasy dirt dyes degree;
The resin that takes a morsel is put into test tube, soaks resin 30 minutes with the 6mol/L concentrated hydrochloric acid, takes out a part of acid solution, to wherein dripping saturated potassium ferrocyanide, determines that resin is subjected to the iron pollution degree;
The resin that takes a morsel is put into test tube, sodium chloride solution immersion treatment with 10% 20-30 minute uses 10%NaCl and 4%NaOH mixed liquor 500ml again under 40 ℃ of conditions, soaks wet resin 24 hours, survey the total organic carbon or the COD of soak, determine that resin is subjected to organic pollution level;
The 3rd step: pollute the resin recovery
According to the second resin stain type that identify of step, pollute, remove iron pollution, remove the order of organic contamination according to oil removing, select according to the processing of recovering successively of following a kind of or more than one methods:
The processing method that A, greasy dirt dye: resin is that 8% NaCl solution is regenerated with concentration earlier, under 40-50 ℃ of temperature, carry out oil removing as resuscitation fluid with 0.1%-0.2% non-ionic surface active agent FL-9, the cumulative volume of resuscitation fluid is 2 times of resin volume, pour out the recovery waste liquid after the processing, the resin after the recovery is clean with pure water rinsing;
The processing method of B, iron pollution: (1) with concentration be 10%, temperature is 40 ± 2 ℃ sodium chloride, and resin was carried out circular treatment 2 hours, the discharging waste liquid, again with desalted water clean 2 hours to water outlet near neutral; (2) with desalted water the negative resin bed is full of, in concentration is 10% hydrochloric acid, adds sodium sulfite, make concentration of sodium sulfite reach 5%, under 40 ± 2 ℃ of temperature, discharge waste liquid after resin circulated 4 hours, with desalted water clean 2 hours to water outlet near neutral;
The processing method of C, organic contamination resin:
The processing method of slight organic contamination: compound concentration is 4% sodium hydroxide solution and 10% sodium chloride solution equal-volume mixed liquor, and allocate the 0.4%Tritonx-100 assistant medicament therein into, form resuscitation fluid, under 40 ℃ condition with resuscitation fluid to resin circular treatment 8-12 hour;
Severe organic is polluted the processing method of resin: allocate effective chlorine density in the equal-volume mixed liquor of 4%NaOH and 10%NaCl into and be and allocate 1% hydrogen peroxide in 0.5% clorox or 4%NaOH and the 10%NaCl equal-volume mixed liquor into and form resuscitation fluid, with resuscitation fluid to the resin processing 4 hours of recovering that circulates.
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CN101612598B (en) * | 2009-07-22 | 2012-05-30 | 重庆汉能环保工程技术有限公司 | Method for recovering polluted resin |
CN102631955B (en) * | 2012-05-04 | 2014-04-23 | 哈尔滨工业大学 | Restoration method for removing iron pollution of anion exchange resin and restoration drug formula |
CN107961819A (en) * | 2017-12-14 | 2018-04-27 | 长沙理工大学 | It is a kind of to be suitable for by the method for resuscitation of the cation exchange resin of lauryl amine pollution |
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CN110564897B (en) * | 2019-08-06 | 2022-03-29 | 四川雅华生物有限公司 | Recovery method and system for ion exchange column in xylose preparation |
CN111282603B (en) * | 2020-03-27 | 2023-03-24 | 安徽银创生物科技股份有限公司 | Regeneration method of waste cation exchange resin |
CN111659363A (en) * | 2020-06-13 | 2020-09-15 | 劲牌有限公司 | Regeneration method of macroporous adsorption resin |
CN111905842A (en) * | 2020-08-21 | 2020-11-10 | 四川省宜宾惠美线业有限责任公司 | Method for treating poisoned anion resin |
CN115870018B (en) * | 2021-09-28 | 2024-08-09 | 中核矿业科技集团有限公司 | Regeneration method of neutral in-situ leaching resin |
CN114314753A (en) * | 2021-12-27 | 2022-04-12 | 湖南金牛化工有限公司 | Alkali-saving type anion bed regeneration treatment method |
CN116237090A (en) * | 2023-02-21 | 2023-06-09 | 华能山东发电有限公司白杨河发电厂 | Method for treating and regenerating negative resin for water treatment |
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JPH10225644A (en) * | 1997-02-13 | 1998-08-25 | Mitsubishi Chem Corp | Method for regenerating strongly basic anion-exchange resin |
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JP2007131467A (en) * | 2005-11-09 | 2007-05-31 | Matsushita Electric Ind Co Ltd | Optical element molding apparatus |
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Patent Citations (3)
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JPH10225644A (en) * | 1997-02-13 | 1998-08-25 | Mitsubishi Chem Corp | Method for regenerating strongly basic anion-exchange resin |
CN1225294A (en) * | 1998-10-15 | 1999-08-11 | 叶贤忠 | Method for reactivation of ion-exchange resin |
JP2007131467A (en) * | 2005-11-09 | 2007-05-31 | Matsushita Electric Ind Co Ltd | Optical element molding apparatus |
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