CN105771885A - Preparation method of modified zeolite and application of modified zeolite in arsenic-bearing waste water - Google Patents
Preparation method of modified zeolite and application of modified zeolite in arsenic-bearing waste water Download PDFInfo
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- CN105771885A CN105771885A CN201610332587.5A CN201610332587A CN105771885A CN 105771885 A CN105771885 A CN 105771885A CN 201610332587 A CN201610332587 A CN 201610332587A CN 105771885 A CN105771885 A CN 105771885A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
Abstract
The invention discloses a preparation method of modified zeolite and application of the modified zeolite in arsenic-bearing waste water. The preparation method of the modified zeolite comprises the following steps: soaking natural zeolite in a hydrochloric acid solution and putting the natural zeolite into a container; adding a ferric chloride solution and a sodium hydroxide solution to the container; and carrying out mixing and reacting to obtain the modified zeolite which is large in specific surface area, high in arsenic adsorption capacity and high in capacity. When the modified zeolite is applied to treatment of the arsenic-bearing waste water, the selective removal rate on arsenic is high, and the treatment cost on the arsenic-bearing waste water is greatly reduced.
Description
Technical field
The present invention relates to the method for modifying of a kind of natural zeolite, be specifically related to the preparation method of a kind of modified zeolite with selective absorption arsenic and the application process in processing arsenic-containing waste water thereof, belong to water treatment field.
Background technology
Arsenic is a kind of toxic element, in the earth's crust main with the indissoluble arsenates such as the calcium of low toxicity, ferrum, manganese, aluminum and Realgar, Orpimentum (Auripigmentum), mispickel sulfides form stable be present in rock stratum and soil.The mankind are in mineral resource development and utilization process, and the natural stability form of arsenic is destroyed and discharged high malicious water solublity arsenic, the high-concentration arsenic-containing wastewater especially produced in nonferrous metallurgical process, have become as one of main path of release high poison arsenic.Recently, there occurs a lot of regional arseniasis event in nonferrous smelting industry City Regions such as China Hunan, Guangxi, Guizhou, Yunnan, arsenic pollutes the tender subject having become as society's extensive concern.Therefore, find a kind of arsenic removal thorough, simple to operate, life with low cost and the dearsenicating method of drinking water, arsenic-containing waste water is processed and purifying of drinking water has realistic meaning, and absorption method is a kind of comparatively ripe and simple wastewater processing technology, the amount of being particularly well-suited to is big and water treatment system that concentration is relatively low.
In conventional several dearsenicating methods, absorption method is because technique is simple, economical and practical, technology maturation and be widely used in processing the aqueous systems relatively low containing arsenic concentration.The method uses the insoluble solid material with large specific surface area as absorption carrier, by the mechanism such as physical absorption, chemisorbed or ion exchange, the arsenic pollutant in water is fixed on adsorbent surface, thus reaching the purpose of arsenic removal.Relative to coagulant sedimentation, absorption method will not introduce new pollutant while removing water pollutant, thus is applicable to drinking water treatment field.
The advantages such as natural zeolite has stable in properties, and specific surface area is big, has good adsorptive selectivity and an ion exchangeable, cheap, are widely used in sewage disposal technology.At present, having the relevant report utilizing natural zeolite arsenic removal, arsenic is had adsorption by natural zeolite, also has part ion exchange interaction.Natural zeolite mainly relies on adsorption for the removal of As (V), and with arsenite ion generation complexation, the removal of As (III) is formed complex mainly by zeolite.But the arsenic removal ability of natural zeolite is poor, mainly natural zeolite internal voids is many containing other impurity, easily forms blocking, affect effect of removing arsenic in adsorption treatment on sewage process.And the process of natural zeolite absorption arsenic in waste water mostly is static adsorption, it is subject to temperature, the impact of the physicochemical properties such as pH so that the arsenic removal cycle is long.
Summary of the invention
For the above-mentioned technical problem existed in prior art, it is an object of the invention to be in that to provide a kind of specific surface area big, and the adsorption capacity of arsenic is big and modified zeolite that selective adsorption capacity is strong preparation method, the method is simple to operate, low cost, it is possible to large-scale production.
Another object of the present invention is to be in that to provide described modified zeolite to apply in arsenic-containing waste water processing procedure, and it is high that modified zeolite has arsenic removal efficiency, and the advantage that selectivity is strong is substantially reduced arsenic-containing waste water processing cost.
In order to realize above-mentioned technical purpose, the preparation method that the invention provides a kind of modified zeolite, the method be by natural zeolite in hydrochloric acid solution after immersion treatment, it is placed in container, in described container, it is simultaneously introduced ferric chloride solution and sodium hydroxide solution, mixing, reaction, to obtain final product.
Preferred scheme, reaction carries out when temperature is 40 DEG C～100 DEG C；Preferably reaction temperature is 60 DEG C～90 DEG C, it is most preferred that be 80 DEG C.
More preferably scheme, the response time is not less than 6h, more preferably 6h～8h,
Preferred scheme, the natural zeolite after immersion treatment is 1:(20～50 with ferric chloride solution and the total solid-to-liquid ratio of sodium hydroxide solution) g/mL；More preferably 1:(40～50) g/mL.
Preferred scheme, the concentration of described ferric chloride solution is 2～3mol/L.
Preferred scheme, the concentration of described sodium hydroxide solution is 4～6mol/L.
Preferred scheme, the volume ratio of described ferric chloride solution and described sodium hydroxide solution is 1:1.
Preferred scheme, concentration of hydrochloric acid solution is 3～6mol/L.
More preferably scheme, described natural zeolite time of immersion treatment in hydrochloric acid solution is 4～6h.
Preferred scheme, after the natural zeolite water cyclic washing after immersion treatment presents neutrality to cleaning mixture, is placed at 105～130 DEG C of temperature, dry 8～16h.
Preferred scheme, after having reacted, reaction gained solid product through in water cyclic washing to cleaning mixture without free iron after, be placed at 105～130 DEG C of temperature, dry 8～16h.
Present invention also offers the application of described preparation method gained modified zeolite, this modified zeolite is applied to selective absorption and removes arsenic in arsenic-containing waste water.
The modified of natural zeolite is adopt HCl treatment in conjunction with ferric chloride-naoh treatment by technical scheme.Natural zeolite processes initially with soak with hydrochloric acid, on the one hand, can effectively be removed by the impurity in zeolite cavity, makes dredging space, increase passage, increasing specific surface area, makes the internal activation of zeolite on the other hand, increases avtive spot, is conducive to follow-up modifiying.Again by the zeolite ferric chloride solution after HCl treatment and sodium hydroxide solution haptoreaction, iron chloride can enter inside zeolite cavity, and internal in duct can react the weakly alkaline hydrated ferric oxide. of generation with sodium hydroxide, hydrated ferric oxide. in-situ deposition is at zeolite cavity inner surface, and the special adsorption making full use of Arsenic By Ferric Hydroxide improves the adsorption selectivity to arsenic.
Hinge structure, the Advantageous Effects that technical scheme is brought.
1, the preparation method of the modified zeolite of the present invention is simple, economical environment-protective, and the relative natural zeolite of modified zeolite of preparation, and specific surface increases, and improves adsorption capacity, and adds the chemisorbed function to arsenic, and the ability of selective absorption arsenic improves.
2, modified zeolite prepared by the present invention is for processing arsenic-containing waste water, the selective absorption efficiency of arsenic is obviously improved, greatly reduces the processing cost to arsenic-containing waste water, have a good application prospect.
Accompanying drawing explanation
[Fig. 1] is the temperature impact on modified zeolite arsenic removal efficiency；
[Fig. 2] is the time impact on modified zeolite arsenic removal efficiency；
[Fig. 3] is modified solution and the impact on modified zeolite arsenic removal efficiency of the zeolite liquid-solid ratio；
[Fig. 4] is natural zeolite arsenic removal efficiency.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is described further, rather than the restriction to the claims in the present invention protection domain.
Embodiment 1
The temperature impact on modified zeolite arsenic removal efficiency:
Weigh natural zeolite, the hydrochloric acid solution of 3mol/L soaks 4h, takes out zeolite, repeatedly rinse with distilled water, until neutral；Zeolite is put in drying baker, dry 4h at 110 DEG C.The zeolite of pretreatment is obtained through acidleach.
Seven groups of parallel tests: weigh the zeolite through pretreatment that quality is 2g, be placed in the conical flask of 250mL, be simultaneously introduced the FeCl of 2.5mol/L respectively3·6H2The NaOH solution 50mL of O solution 50mL and 5mol/L, after being sufficiently mixed, is put in water-bath by conical flask, and being respectively provided with temperature is 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, reacts 6h.Zeolite is taken out, repeatedly rinses with distilled water, to solution, there is no iron ion.Zeolite is put in drying baker, be dried at 120 DEG C of temperature, namely obtain modified zeolite.Seven groups of modified zeolites carry out arsenic removal experiment respectively, and the temperature obtained is on the impact of zeolite arsenic removal efficiency as shown in Figure 1.
The configuration of arsenic solution: adopt the arsenic containing solution of 12 hydration natrium arsenicum preparation arsenic content 6mg/L.
2g modified zeolite, adds 250mL conical flask, adds 100mL arsenic containing solution, is placed on constant temperature oscillator by conical flask, and pH regulator is to the speed of 7,170r/min, at 25-30 DEG C, shakes 10h, filters, utilize in ICP filtrates tested containing arsenic concentration.
The calculating of arsenic removal efficiency:
Clearance η=(Co-C)/Co× 100%
In formula: C represents the arsenic concentration after zeolite adsorption in water sample；
C0Represent the initial concentration of arsenic.
As seen from Figure 1, when liquid-solid ratio and time are certain, when temperature is 80 DEG C, the arsenic removal of modified zeolite is most effective, can reach 81.23%.
Embodiment 2
The time impact on modified zeolite arsenic removal efficiency:
Weigh the natural zeolite of certain mass, the hydrochloric acid solution of 3mol/L soaks 4h, takes out zeolite, repeatedly rinse with distilled water, until neutral；Zeolite is put in drying baker, dry 4h at 110 DEG C.The zeolite of pretreatment is obtained through acidleach.
Seven groups of parallel tests: weigh the zeolite through pretreatment that quality is 2g, be placed in the conical flask of 250mL, be separately added into the FeCl of 2.5mol/L3·6H2The NaOH solution 50mL of O solution 50mL and 5mol/L, after being sufficiently mixed, is put in water-bath by conical flask, and arranging temperature is 80 DEG C, the response time respectively 2,3,4,5,6,7,8h.Zeolite is taken out, repeatedly rinses with distilled water, to solution, there is no iron ion.Zeolite is put in drying baker, be dried at 120 DEG C of temperature, namely obtain modified zeolite.Seven groups of modified zeolites carry out arsenic removal experiment respectively, and the impact such as Fig. 2 of the modification time stone arsenic removal efficiency obtained shows.
The configuration of arsenic solution: adopt the arsenic containing solution of 12 hydration natrium arsenicum preparation arsenic content 6mg/L.
2g modified zeolite, adds 250mL conical flask, adds 100mL arsenic containing solution, is placed on constant temperature oscillator by conical flask, and pH regulator is to the speed of 7,170r/min, at 25-30 DEG C, shakes 10h, filters, utilize in ICP filtrates tested containing arsenic concentration.
The calculating of arsenic removal efficiency:
Clearance η=(Co-C)/Co× 100%
In formula: C represents the arsenic concentration after zeolite adsorption in water sample；
C0Represent the initial concentration of arsenic.
As seen from Figure 2, when identical temperature and liquid-solid ratio, when the time is 6h, the arsenic removal of modified zeolite is most effective, can reach 71.27%.
Embodiment 3
Modified solution and the impact on modified zeolite arsenic removal efficiency of the zeolite liquid-solid ratio:
Weigh the natural zeolite of certain mass, the hydrochloric acid solution of 3mol/L soaks 4h, takes out zeolite, repeatedly rinse with distilled water, until neutral；Zeolite is put in drying baker, dry 4h at 110 DEG C.The zeolite of pretreatment is obtained through acidleach.
Seven groups of parallel tests: weigh the zeolite through pretreatment that quality is 2g, be placed in the conical flask of 250mL, being separately added into mol ratio is 1；The FeCl of the 2.5mol/L of 23·6H2The NaOH solution of O solution and 5mol/L, the cumulative volume of modification liquid respectively 20,40,60,70,80,90,100mL be sufficiently mixed after, conical flask is put in water-bath, arranging temperature is 80 DEG C, and the response time is 6h respectively.Zeolite is taken out, repeatedly rinses with distilled water, to solution, there is no iron ion.Zeolite is put in drying baker, be dried at 120 DEG C of temperature, namely obtain modified zeolite.Seven groups of modified zeolites carry out arsenic removal experiment respectively, and the impact such as Fig. 3 of the modification time stone arsenic removal efficiency obtained shows.
The configuration of arsenic solution: adopt the arsenic containing solution of 12 hydration natrium arsenicum preparation arsenic content 6mg/L.
2g modified zeolite, adds 250mL conical flask, adds 100mL arsenic containing solution, is placed on constant temperature oscillator by conical flask, and pH regulator is to the speed of 7,170r/min, at 25-30 DEG C, shakes 10h, filters, utilize in ICP filtrates tested containing arsenic concentration.
The calculating of arsenic removal efficiency:
Clearance η=(Co-C)/Co× 100%
In formula: C represents the arsenic concentration after zeolite adsorption in water sample；
C0Represent the initial concentration of arsenic.
As seen from Figure 3, when temperature and time is certain, when modification liquid cumulative volume is 80mL, the arsenic removal efficiency of modified zeolite, 82.61% can be reached, along with the increase of modification liquid cumulative volume, arsenic removal efficiency does not significantly improve.
Comparative example 1
The unmodified natural zeolite adsorption experiment to arsenic:
The configuration of arsenic solution: adopt the arsenic containing solution of 12 hydration natrium arsenicum preparation arsenic content 6mg/L.
Taking modified zeolite, add 250mL conical flask, add 100mL arsenic containing solution, be placed on constant temperature oscillator by conical flask, pH regulator is to the speed of 7,170r/min, at 25-30 DEG C, shakes 10h, filters, utilize in ICP filtrates tested containing arsenic concentration.
The calculating of arsenic removal efficiency:
Clearance η=(Co-C)/Co× 100%
In formula: C represents the arsenic concentration after zeolite adsorption in water sample；
C0Represent the initial concentration of arsenic.
Seven groups of parallel tests: weigh respectively quality be 1,1.5,2,2.5,3,3.5,4,4.5, the natural zeolite of 5g, carry out containing arsenic adsorption experiment.Adsorption efficiency is as shown in Figure 4.
Claims (10)
1. the preparation method of a modified zeolite, it is characterised in that: natural zeolite after immersion treatment, is placed in container in hydrochloric acid solution, in described container, is simultaneously introduced ferric chloride solution and sodium hydroxide solution, mixing, reaction, to obtain final product.
2. the preparation method of modified zeolite according to claim 1, it is characterised in that: described reaction carries out when temperature is 40 DEG C～100 DEG C.
3. the preparation method of modified zeolite according to claim 2, it is characterised in that: the response time is for being not less than 6h.
4. the preparation method of modified zeolite according to claim 1, it is characterised in that:
Natural zeolite after immersion treatment is 1:(20～50 with ferric chloride solution and the total solid-to-liquid ratio of sodium hydroxide solution) g/mL；
The concentration of described ferric chloride solution is 2～3mol/L；
The concentration of described sodium hydroxide solution is 4～6mol/L；
The volume ratio of described ferric chloride solution and described sodium hydroxide solution is 1:1.
5. the preparation method of modified zeolite according to claim 4, it is characterised in that: the natural zeolite after immersion treatment is 1:(40～50 with ferric chloride solution and the total solid-to-liquid ratio of sodium hydroxide solution) g/mL.
6. the preparation method of modified zeolite according to claim 1, it is characterised in that: described concentration of hydrochloric acid solution is 3～6mol/L.
7. the preparation method of the modified zeolite according to claim 1 or 6, it is characterised in that: described natural zeolite time of immersion treatment in described hydrochloric acid solution is 4～6h.
8. the preparation method wanting modified zeolite described in 1 or 6 according to right, it is characterised in that: the natural zeolite use water cyclic washing after immersion treatment is placed at 105～130 DEG C of temperature after being neutrality to cleaning mixture, dry 8～16h.
9. the preparation method of modified zeolite according to claim 1, it is characterised in that: after having reacted, reaction gained solid product through in water cyclic washing to cleaning mixture without free iron after, be placed at 105～130 DEG C of temperature, dry 8～16h.
10. the application of the preparation method gained modified zeolite according to claim 1～6,9 any one, it is characterised in that: it is applied to selective absorption and removes arsenic in arsenic-containing waste water.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811200A (en) * | 2017-01-13 | 2017-06-09 | 环保桥（湖南）生态环境修复有限公司 | A kind of complex repairation agent for reducing arsenic content in the crops of arsenic pollution area and preparation method thereof |
| CN107020066A (en) * | 2017-04-06 | 2017-08-08 | 湖南三友环保科技股份有限公司 | The preparation method and application of load hydrogen ferric oxide nano zeolitic material |
| CN107970886A (en) * | 2017-11-09 | 2018-05-01 | 广东工业大学 | A kind of graphene oxide and the composite modified zeolite filler of iron chloride and preparation method thereof |
| CN108372202A (en) * | 2018-04-03 | 2018-08-07 | 格丰科技材料有限公司 | A method of the reparation medicament for administering heavy-metal contaminated soil and its improvement heavy-metal contaminated soil |
| CN109095631A (en) * | 2017-06-21 | 2018-12-28 | P&I人类韩国有限公司 | The mixing sewerage system overflow and non-point pollution source processing system of oil removal, phosphorus and heavy metal can be removed simultaneously |
| CN110372075A (en) * | 2019-05-14 | 2019-10-25 | 山东环瑞生态科技有限公司 | A kind of new and effective fluorine removal medicament and its application |
| CN113893818A (en) * | 2021-10-04 | 2022-01-07 | 广州东智盟化妆品有限公司 | Surface-modified zeolite, linaloe essential oil for slimming, extraction method and application |
| CN114409132A (en) * | 2022-01-18 | 2022-04-29 | 常州大学 | Crystal glass production wastewater quality-based pretreatment device and method |
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| CN106811200A (en) * | 2017-01-13 | 2017-06-09 | 环保桥（湖南）生态环境修复有限公司 | A kind of complex repairation agent for reducing arsenic content in the crops of arsenic pollution area and preparation method thereof |
| CN106811200B (en) * | 2017-01-13 | 2020-04-24 | 环保桥（湖南）生态环境修复有限公司 | Composite repairing agent for reducing arsenic content in crops in arsenic-polluted area and preparation method thereof |
| CN107020066A (en) * | 2017-04-06 | 2017-08-08 | 湖南三友环保科技股份有限公司 | The preparation method and application of load hydrogen ferric oxide nano zeolitic material |
| CN109095631B (en) * | 2017-06-21 | 2022-03-15 | P&I人类韩国有限公司 | Mixed sewer overflow and non-point pollution source treatment system capable of simultaneously removing suspended matters, phosphorus and heavy metals |
| CN109095631A (en) * | 2017-06-21 | 2018-12-28 | P&I人类韩国有限公司 | The mixing sewerage system overflow and non-point pollution source processing system of oil removal, phosphorus and heavy metal can be removed simultaneously |
| CN107970886A (en) * | 2017-11-09 | 2018-05-01 | 广东工业大学 | A kind of graphene oxide and the composite modified zeolite filler of iron chloride and preparation method thereof |
| CN107970886B (en) * | 2017-11-09 | 2023-10-27 | 广东工业大学 | Graphene oxide and ferric chloride composite modified zeolite filter material and preparation method thereof |
| CN108372202A (en) * | 2018-04-03 | 2018-08-07 | 格丰科技材料有限公司 | A method of the reparation medicament for administering heavy-metal contaminated soil and its improvement heavy-metal contaminated soil |
| CN110372075B (en) * | 2019-05-14 | 2022-03-25 | 山东环瑞生态科技有限公司 | Efficient defluorination medicament and application thereof |
| CN110372075A (en) * | 2019-05-14 | 2019-10-25 | 山东环瑞生态科技有限公司 | A kind of new and effective fluorine removal medicament and its application |
| CN113893818A (en) * | 2021-10-04 | 2022-01-07 | 广州东智盟化妆品有限公司 | Surface-modified zeolite, linaloe essential oil for slimming, extraction method and application |
| CN113893818B (en) * | 2021-10-04 | 2024-04-26 | 广州东智盟化妆品有限公司 | Surface-modified zeolite, agilawood essential oil for slimming, extraction method and application |
| CN114409132A (en) * | 2022-01-18 | 2022-04-29 | 常州大学 | Crystal glass production wastewater quality-based pretreatment device and method |
| CN114409132B (en) * | 2022-01-18 | 2023-11-03 | 常州大学 | Device and method for separate pretreatment of waste water from crystal glass production |
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