CN101920190A - Zeolite modifying method and application thereof in removing arsenic in water - Google Patents
Zeolite modifying method and application thereof in removing arsenic in water Download PDFInfo
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- CN101920190A CN101920190A CN 201010203314 CN201010203314A CN101920190A CN 101920190 A CN101920190 A CN 101920190A CN 201010203314 CN201010203314 CN 201010203314 CN 201010203314 A CN201010203314 A CN 201010203314A CN 101920190 A CN101920190 A CN 101920190A
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Abstract
The invention belongs to the technical field of water treatment and in particular relates to a novel adsorbing material prepared by modifying cheap nonmetallic minerals-zeolite ores. The material is suitable for remediation of arsenic pollution of the water body. The material can effectively adsorb arsenic in the arsenic-polluted water body and reduce the content of arsenic in the water body and has great significance in solving the problem of arsenic pollution of the water body and realizing recycling of the waste resources. The invention is characterized in that the modified zeolite adsorbing material comprises the following components by weight according to 100kg of dry basis of the prepared product: 97-99.7kg of natural zeolite powder (sieved by 200-mesh sieves) and 0.3-3kg of nano TiO2. The invention also discloses a preparation method and application of the modified zeolite adsorbing material.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of Zeolite modifying method and the purposes in the water body arsenic removal thereof.The present invention is a raw material with a kind of novel environment friendly nonmetallic mineral material zeolite ore deposit cheap and easy to get, and it is carried out modification, and is used for arsenic in the adsorbed water body.Zeolite of the present invention ore deposit modification technology can make the zeolite ore deposit after the modification use as the water body arsenic adsorbent material, removes the arsenic in the water body efficiently, and the pollution problem that solves arsenic in the water body is had crucial meaning.
Technical background
Arsenic and arsenic compound are the carcinogenic substances of generally acknowledging.Because mining, sewage irrigation and digging well to get water such as drink at activity, arsenic compound dissolves in underground water and the surface water in a large number in the epigeosphere, has brought serious water body arsenic contamination problem.Environment mineral material handle on the method for arsenic contamination have easy acquisition, cost is low, effective and be not prone to advantage such as secondary pollution and reusable edible and more and more be subject to people's attention.Utilize environment mineral material to remove arsenic in the water body, the ore that will discard originally effectively utilizes on the one hand, has played the effect of turning waste into wealth; On the other hand, the arsenic of removing in the water body with environment mineral material can not cause secondary pollution, greatly reduces processing cost and subsequent treatment complexity.
By retrieval, the application for a patent for invention of the environment mineral material that arsenic is handled in the Chinese invention patent relates to multiple nonmetal and metalliferous minerals such as zeolite.Present by retrieval relevant patent documentation is as follows:
Application number provides the cleanser of a kind of arsenic and heavy metal wastewater thereby for 89109581 document, by magnalium janosite, molecular formula be (Fe, Mg) (Fe, Al)
[4](SO
[4])
[6](OH)
[2]2OH
[2]O and unformed charcoal cooperate composition with 1: 1～4 weight ratio.Wherein the magnalium janosite adopts vitriol lixiviation limonite manufactured.Also contain 2～8% active silica in the product; Unformed charcoal is the natural activity charcoal, is formed by unformed charcoal and a small amount of landwaste, is lost " the dignified limestone in carbonaceous volcano " at present to be emanated through hydrolysis make.
Application number provides a kind of method and apparatus that extracts arsenic from arsenic-containing waste water for 94110419 document.Undertaken by following step, promptly filter its suspension; Regulate its pH value less than 1.5; By device reaction device and ferrous sulfide reaction; Use isolation technics and extract arsenic; With in the milk of lime and waste water, control pH value through precipitate and separate, makes the water quality arsenic content less than 0.5mg/L between 8-9, bears divalent sulfur content less than 1mg/L.The arsenic rate of recovery reaches more than 99.5%, arsenic sulfide arsenic content size 50%.Can prevent the pollution of arsenic effectively, reduce cost, for the comprehensive utilization of arsenic resource provides a new way environment.
Application number is the method that 00131216 document finds to remove arsenic in the Drinking Water, lead, chromium, cadmium, mercury, is NaOH and bleaching essence or the bleaching powder that adds ferrous sulfate, adjust pH in the Drinking Water that contains this five heavy metal species successively.After the present invention was added to the water above-mentioned substance, bleaching is smart to be oxidized to high valence state with five elements and part iron, generated infusibility hydroxide or infusibility salt precipitation in water, and they are removed to be filtered by absorption of the hydroxide floccule of iron and co-precipitation.Adopt the inventive method can effectively remove arsenic, lead, chromium, cadmium, mercury, make the content of iron in the water, arsenic, lead, chromium, cadmium be significantly less than national standard.
Application number provides a kind of method of removing arsenic and fluoride in same process from the aqueous solution for 01815105 document.Specifically, the pH with the described aqueous solution is adjusted to about 5-8.The composition of adding calcium salt and iron or aluminium salt contain the insoluble solid of arsenic and fluoride with formation.From the described aqueous solution, remove described solid then.
Application number is that 200480003018 document is removed arsenic by following method from water and other water-containing materials: (1) is with containing+compound of 4 oxidation state ceriums, preferred ceria material handling, be oxidized to+arsenic of 5 oxidation state with arsenic+3 oxidation state, (2) usually by make the material handled with aluminium oxide or contain+cationic other precipitating reagents of 3 oxidation state contact, remove+arsenic of 5 oxidation state from aqueous phase.
Application number is composite adsorbing material of removing in 200510027898 the document arsenic in the water and preparation method thereof, relates to a kind of arsenic-removing adsorption agent and preparation method.The arsenic adsorbance of the composite adsorbing material of the present invention that is composited by active carbon and iron oxide be active carbon 2-5 doubly.Active carbon after will washing earlier is incubated 24 hours down at 90 ℃, drying.Add then in the nitric acid, stir, place after 4 hours, washing, and stand-by at 95～100 ℃ times dry 24 hours.With FeSO
47H
2O and FeCl
36H
2After O is dissolved in water, add among the NaOH of 5mol/L, stir, generate iron oxide precipitation, be titrated to pH value of solution=9～10 with NaOH at 70 ℃; Wash with water, add laurate again, drip NaOH simultaneously, stirred 10 minutes, be heated to 90 ℃, constant temperature 30 minutes.Adjust pH=4～5.Active carbon is mixed with iron oxide suspension, stir and to make high power capacity of the present invention, high selectivity and high adsorption rate, high mechanical properties, renewable and composite adsorbing material cheaply.Technology of the present invention is simple, and is easy to operate, and the sludge silt generation is few.Can effectively remove arsenic or other heavy metals in the water.
Mostly above-mentioned patent documentation is the processing at arsenic in waste water and the drinking water, and still rare for the removal technology and the material of arsenic from underwater, does not see patent application as yet in particular for the permeable reactive wall material of Arsenic Contamination in Groundwater reparation.Therefore, the present invention repairs significant for arsenic contamination underground water.
Summary of the invention
The objective of the invention is to overcome the defective of prior art, seek a kind of preparation method of sorbing material of removal water body arsenic of high-efficiency and economic, utilize the modification of zeolite ore deposit is handled, make a kind of can adsorbed water body in the new material of arsenic.Purpose of the present invention also comprises the application of this arsenic removal material.The modified zeolite pit wood material of the present invention preparation is to the clearance height of arsenic in the water body, non-secondary pollution, and regenerability is good, satisfies the needs that current removal water body arsenic is up to state standards.
The present invention is achieved in that
The present invention is based on nano-TiO
2The characteristic of efficient arsenic-adsorbing and natural zeolite ore is set out, on the basis of the various natural zeolite ores of screening, natural zeolite ore with the Hubei city is a major ingredient, be aided with butyl titanate, absolute ethyl alcohol is a modifier, by technologies such as material mixing, stirring, hydrolysis, washing and drying, roastings, be prepared into modified zeolite (its preparation technology and technology path are referring to Fig. 1).Implementing core technology of the present invention is by utilizing the strong adsorption capacity of zeolite, butyl titanate is fixed on the zeolite and forms stabilized nano titanium dioxide by hydrolysis, drying roasting then is fixed on nano titanium oxide on zeolite surface and the endoporus, the effect of arsenic removal is relatively determined a kind of modification technology of zeolite ore deposit of the best.
Concrete technical scheme of the present invention is:
A kind of zeolite ore deposit method of modifying, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (90% crosses 100 orders) 97～99.7kg;
Nano-TiO
20.3～3kg;
Prepare according to the following step:
1) takes by weighing butyl titanate by formula ratio, be dissolved in the absolute ethyl alcohol, stirred butyl titanate-alcoholic solution 30 minutes;
2) take by weighing natural zeolite by formula ratio, pour in step 1) gained butyl titanate-alcoholic solution, in agitator, stirred 1 hour;
3) slowly add distilled water in the solution that will evenly stir at a slow speed, to forming gel;
4) gel is dried down at 100 ℃, spend distilled water flushing again 2 times after the grinding evenly;
5) modified zeolite after the flushing is put into baking oven 100 ℃ of oven dry down, puts into Muffle furnace again 300 ℃ of following roastings 2 hours;
6) gained modified zeolite cooling back is standby.
According to aforesaid preparation method, one of prioritization scheme wherein, component by weight is as follows:
A kind of zeolite ore deposit method of modifying, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (crossing 200 orders) 97～99.7kg;
Nano-TiO
20.3～3kg.
According to aforesaid preparation method, two of prioritization scheme wherein, component by weight is as follows:
A kind of zeolite ore deposit method of modifying, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (90% crosses 100 orders) 98～99.5kg;
Nano-TiO
20.5-2kg.
According to aforesaid preparation method, three of prioritization scheme wherein, component by weight is as follows:
A kind of zeolite ore deposit method of modifying, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (90% crosses 100 orders) 99kg;
Nano-TiO
21kg.
The TiO of the present invention's preparation
2The modified zeolite material is fine to the clearance of water body arsenic.Result of study shows, at the water body arsenic concentration is 1mg/L, adsorbent/water ratio is 3g/L, the adsorption reaction time is under the 90min condition, the residual concentration of As (III) and As (V) only is 4.36 and 2.10 μ g/L, be lower than the standard of the drinking water arsenic＜10 μ g/L of national regulation, and modified zeolite 7.64mg/g and 6.59mg/g (see figure 3) have been reached respectively to the saturated adsorption capacity of As (III) and As (V).In view of the above, the 1kg modified zeolite can be removed 6.5～7.6g arsenic in the water, and to the high concentration arsenic-containing waste water of 1mg/L, the 1kg modified zeolite can be handled 5～8m
3According to another the market constant price, the cost RMB that preparation 100kg modified zeolite needs only is 110 yuan, and than the 35000 yuan/100kg of price of pure nano titanium oxide sorbing material, this method of modifying can reduce cost greatly.To sum up, the made arsenic adsorbent material of the present invention has very high cost performance.
The material of the present invention preparation has good regeneration effect, with 0.1mol/L NaOH to inhaling the TiO behind the arsenic
2Modified zeolite ore deposit desorb 24h, desorption efficiency reaches more than 70%, simultaneously Zai Sheng TiO
2The zeolite ore deposit of modification still can reach more than 80% As (V) clearance.
Know-why of the present invention is:
Excellent properties such as that the zeolite ore deposit has is high temperature resistant, corrosion-resistant, high strength, strong absorption, strong ion exchangeable, environmental pollution are widely used in each field such as agricultural, animal husbandry, light industry and environmental protection.Titanium dioxide is a kind of catalyst of stable environmental protection, and better to the adsorption effect of arsenic in the water body.Xiao Yabing etc. (2003) studies show that nano-TiO
2As (III) and As (V) there is bigger adsorption capacity.Although TiO
2Effect of removing arsenic is good, but because it costs an arm and a leg, particle diameter is too small, makes it that certain limitation be arranged in actual applications.By contrast, low far away other the similar sorbing materials of zeolite ore deposit price, and the zeolite specific area is big, extraordinary adsorptivity and ion exchangeable.If utilize the strong absorption property of zeolite, firmly be adsorbed on butyl titanate in surface, zeolite ore deposit and the duct and hydrolysis formation stabilized nano TiO
2Method, the zeolite ore deposit is carried out can reaching desirable effect of removing arsenic after a series of modification, and zeolite ingredient and TiO
2(being a kind of safe and reliable food additives) is without any side effects to organism, and this will administer the water body arsenic contamination has crucial meaning.
The invention has the beneficial effects as follows:
1) TiO of the present invention
2Modified zeolite ore deposit preparation process is very simple, major ingredient and modifier is mixed, soaks the hydrolysis washing get final product, and energy consumption is low and cost of material is low;
2) the present invention has taken into full account the desorb and the regeneration problem in modified zeolite ore deposit, makes the modified zeolite ore deposit to use repeatedly, and important meaning is arranged in actual engineering application;
3) the zeolite ore deposit after the modification of the present invention increases significantly to the adsorption capacity of arsenic.
Description of drawings
Fig. 1: technology of the present invention and technology path flow chart.
Fig. 2: the present invention is under experiment condition, and the modified zeolite of natural zeolite and embodiment 1, embodiment 2, embodiment 3 preparations is to the effect of removing arsenic block diagram of simulation arsenic-containing waste water.Fig. 2 shows that material of the present invention can make the arsenic content in the arsenic-containing waste water significantly reduce.
Fig. 3: the present invention is under experiment condition, and the modified zeolite of natural zeolite and embodiment 1, embodiment 2, embodiment 3 preparations is to the adsorption capacity figure of arsenic.Can find that from this figure modification can be brought up to 7.64mg/g and 6.59mg/g to the adsorption capacity of As (III) and As (V) from 0.73mg/g and 1.05mg/g with natural zeolite, has improved 10 times and 6 times respectively.
Fig. 4: the present invention under experiment condition, the curve map of the zeolite adsorption material adsorbed water body arsenic effect temperature influence of invention.Fig. 4 shows that water temperature is to not influence of material arsenic-adsorbing of the present invention.
Fig. 5: the present invention under experiment condition, the curve map that the zeolite adsorption material adsorbed water body arsenic effect of invention is influenced by pH.Fig. 5 shows, in pH was 4～10 scope, pH was to not influence of material arsenic-adsorbing of the present invention.
The specific embodiment
Embodiment 1
A kind of zeolite ore deposit method of modifying, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (90% crosses 100 orders) 97～99.7kg;
Nano-TiO
20.3～3kg;
1, takes by weighing butyl titanate, be dissolved in the absolute ethyl alcohol, stirred 30 minutes;
2, take by weighing natural zeolite, pour in step 1 gained butyl titanate-alcoholic solution, in agitator, stirred 1 hour;
3, slowly add distilled water in the solution that will evenly stir at a slow speed, to forming gel;
4, gel is dried down at 100 ℃, use distilled water flushing again 2 times after the grinding evenly;
5, the modified zeolite after the flushing is put into baking oven 100 ℃ of oven dry down, puts into Muffle furnace again 300 ℃ of following roastings 2 hours;
6, the cooling of gained modified zeolite is standby.
The prepared material of present embodiment is under laboratory condition, arsenic simulated wastewater with 1000 μ g/L of As (III)/As (V) standard reserving solution preparation is adsorbed, make its adsorption rate to As (III) bring up to 99.16% by 9.15% of former natural zeolite (200 order), As (III) drops to 8.38 μ g/L; And the adsorption rate of As (V) is brought up to 99.34% by 7.08%, As (V) concentration drops to 6.62 μ g/L.(referring to Fig. 2)
Embodiment 2
According to the preparation method of embodiment, present embodiment is the prescription of wherein another optimization, and component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (crossing 200 orders) 98～99.5kg;
Nano-TiO
20.5～2kg.
The prepared material of present embodiment is under laboratory condition, arsenic simulated wastewater with 1000 μ g/L of As (III)/As (V) standard reserving solution preparation is adsorbed, make its adsorption rate to As (III) bring up to 99.28% by 9.15% of former natural zeolite (200 order), As (III) drops to 7.18 μ g/L; And the adsorption rate of As (V) is brought up to 99.43% by 7.08%, As (V) concentration drops to 5.75 μ g/L.(referring to Fig. 2)
Embodiment 3
Present embodiment is a preferred forms of the present invention, and according to the preparation method of embodiment, its prescription component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore (crossing 200 orders) 99kg;
Nano-TiO
21kg.
The prepared material of present embodiment is under laboratory condition, arsenic simulated wastewater with 1000 μ g/L of As (III)/As (V) standard reserving solution preparation is adsorbed, make its adsorption rate to As (III) bring up to 99.56% by 9.15% of former natural zeolite (200 order), As (III) drops to 4.36 μ g/L; And the adsorption rate of As (V) is brought up to 99.79% by 7.08%, As (V) concentration drops to 2.10 μ g/L.(referring to Fig. 2)
According to technology provided by the invention and embodiment, the arsenic-adsorbing material that the present invention makes is 200 order zeolite powders of immobilized nano TiO 2, and high concentration water body arsenic is had good effect of removing.If be used to contain the low-concentration arsenic drinking water treatment, during use this sorbing material placed in the clarifier to get final product; If be used to contain the underground water or the industrial wastewater of High Concentration of Arsenic, this material placed in the corresponding treating apparatus get final product.Nano-TiO
2Be non-dissolution type material, in degradable organic pollutant and sterilization, self does not decompose, not stripping, photocatalysis is lasting, and have lasting sterilization, a degradation of contaminant effect, and water body pH do not had influence (seeing Table 1), and sorbing material arsenic-adsorbing of the present invention is not subjected to the influence (seeing Fig. 4 and Fig. 5) of natural temperature and acid-base value substantially, and Practical Performance is strong.
Ti concentration (mg/L) and PH variation in the solution before and after table 1 absorption
Claims (4)
1. Zeolite modifying method, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore is crossed 200 orders, 97～99.7kg;
Nano TiO 2 0.3～3kg;
Prepare according to the following step:
1) takes by weighing butyl titanate by formula ratio, be dissolved in the absolute ethyl alcohol, stirred 30 minutes, obtain butyl titanate-alcoholic solution;
2) take by weighing natural zeolite by formula ratio, pour in step 1) gained butyl titanate-alcoholic solution, in agitator, stirred 1 hour;
3) at a slow speed evenly under the stirring condition, in solution, slowly add and remove distilled water, to forming gel;
4) gel is dried down at 100 ℃, spend distilled water flushing again 2 times after the grinding evenly;
5) modified zeolite after the flushing is put into baking oven 100 ℃ of oven dry down, puts into Muffle furnace again 300 ℃ of following roastings 2 hours;
6) gained modified zeolite cooling back is standby.
2. a kind of Zeolite modifying method according to claim 1, component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore is crossed 200 orders, 98～99.5kg;
Nano TiO 2 0.5～2kg.
3. a kind of zeolite according to claim 1 ore deposit method of modifying is characterized in that component by weight is as follows:
In the manufactured goods butt is 100kg:
Natural zeolite ore is crossed 200 order 99kg;
Nano TiO 2 1kg.
4. each described method application in the removing arsenic from water material of claim 1-3.
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|---|---|---|---|
| CN2010102033143A CN101920190B (en) | 2010-06-12 | 2010-06-12 | Zeolite modifying method and application thereof in removing arsenic in water |
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|---|---|---|---|
| CN2010102033143A CN101920190B (en) | 2010-06-12 | 2010-06-12 | Zeolite modifying method and application thereof in removing arsenic in water |
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| CN101920190B CN101920190B (en) | 2012-05-23 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103084221A (en) * | 2013-02-21 | 2013-05-08 | 中国林业科学研究院亚热带林业研究所 | Method for improving ion-exchange capacity and efficiency of natural zeolite |
| CN103648984A (en) * | 2012-06-14 | 2014-03-19 | 松下电器产业株式会社 | Method for treating arsenic-containing aqueous solution |
| CN106179632A (en) * | 2016-07-14 | 2016-12-07 | 无锡普爱德环保科技有限公司 | A kind of molecular sieve nanometer wet grinding method made as desiccant wheel |
| US9802841B2 (en) | 2012-06-14 | 2017-10-31 | Panasonic Intellectual Property Management Co., Ltd. | Method for treating hexavalent chromium-containing aqueous solution |
| CN108136362A (en) * | 2015-08-14 | 2018-06-08 | 巴斯夫公司 | Adsorbent and the method for manufacturing and using adsorbent |
| CN110280214A (en) * | 2019-06-27 | 2019-09-27 | 西安建筑科技大学 | A kind of permeable coefficient tensor composite material and preparation method and application |
| CN112717992A (en) * | 2020-11-23 | 2021-04-30 | 中国矿业大学(北京) | Manganese-titanium composite modified zeolite and application thereof |
| CN117003328A (en) * | 2023-09-21 | 2023-11-07 | 生态环境部环境规划院 | Odor control agent for wastewater treatment of pesticide contaminated sites and preparation method thereof |
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2010
- 2010-06-12 CN CN2010102033143A patent/CN101920190B/en not_active Expired - Fee Related
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| 《分析科学学报》 20030430 肖亚兵 等 纳米二氧化钛对砷(III）和砷(V)吸附性能的研究 1-4 第19卷, 第2期 2 * |
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|---|---|---|---|---|
| CN103648984A (en) * | 2012-06-14 | 2014-03-19 | 松下电器产业株式会社 | Method for treating arsenic-containing aqueous solution |
| CN103648984B (en) * | 2012-06-14 | 2017-02-22 | 松下知识产权经营株式会社 | Method for treating arsenic-containing aqueous solution |
| US9586844B2 (en) | 2012-06-14 | 2017-03-07 | Panasonic Intellectual Property Management Co., Ltd. | Method for treating arsenic-containing aqueous solution |
| US9802841B2 (en) | 2012-06-14 | 2017-10-31 | Panasonic Intellectual Property Management Co., Ltd. | Method for treating hexavalent chromium-containing aqueous solution |
| CN103084221A (en) * | 2013-02-21 | 2013-05-08 | 中国林业科学研究院亚热带林业研究所 | Method for improving ion-exchange capacity and efficiency of natural zeolite |
| CN108136362A (en) * | 2015-08-14 | 2018-06-08 | 巴斯夫公司 | Adsorbent and the method for manufacturing and using adsorbent |
| CN108136362B (en) * | 2015-08-14 | 2022-01-11 | 巴斯夫公司 | Adsorbents and methods of making and using adsorbents |
| CN106179632A (en) * | 2016-07-14 | 2016-12-07 | 无锡普爱德环保科技有限公司 | A kind of molecular sieve nanometer wet grinding method made as desiccant wheel |
| CN106179632B (en) * | 2016-07-14 | 2018-04-13 | 无锡普爱德环保科技有限公司 | A kind of molecular sieve nanometer wet grinding method made as desiccant wheel |
| CN110280214A (en) * | 2019-06-27 | 2019-09-27 | 西安建筑科技大学 | A kind of permeable coefficient tensor composite material and preparation method and application |
| CN112717992A (en) * | 2020-11-23 | 2021-04-30 | 中国矿业大学(北京) | Manganese-titanium composite modified zeolite and application thereof |
| CN117003328A (en) * | 2023-09-21 | 2023-11-07 | 生态环境部环境规划院 | Odor control agent for wastewater treatment of pesticide contaminated sites and preparation method thereof |
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| CN101920190B (en) | 2012-05-23 |
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