CN100509137C - Preparation of iron-managanese compounded oxide/diatomite adsorbant, using and regenerating method thereof - Google Patents
Preparation of iron-managanese compounded oxide/diatomite adsorbant, using and regenerating method thereof Download PDFInfo
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- CN100509137C CN100509137C CNB2006100081358A CN200610008135A CN100509137C CN 100509137 C CN100509137 C CN 100509137C CN B2006100081358 A CNB2006100081358 A CN B2006100081358A CN 200610008135 A CN200610008135 A CN 200610008135A CN 100509137 C CN100509137 C CN 100509137C
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000001172 regenerating effect Effects 0.000 title description 3
- 239000000243 solution Substances 0.000 claims abstract description 22
- 239000003463 adsorbent Substances 0.000 claims abstract description 12
- 238000001179 sorption measurement Methods 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 6
- 239000012266 salt solution Substances 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 10
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- 238000003483 aging Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 238000009418 renovation Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 claims description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 150000001447 alkali salts Chemical class 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims 2
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims 1
- 239000005909 Kieselgur Substances 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 230000029087 digestion Effects 0.000 claims 1
- 229960002089 ferrous chloride Drugs 0.000 claims 1
- 239000011790 ferrous sulphate Substances 0.000 claims 1
- 235000003891 ferrous sulphate Nutrition 0.000 claims 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 claims 1
- 229940072033 potash Drugs 0.000 claims 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims 1
- 235000015320 potassium carbonate Nutrition 0.000 claims 1
- 235000011118 potassium hydroxide Nutrition 0.000 claims 1
- 230000007420 reactivation Effects 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 229910052785 arsenic Inorganic materials 0.000 abstract description 32
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 32
- 238000010521 absorption reaction Methods 0.000 abstract description 13
- 238000011069 regeneration method Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 10
- 230000008929 regeneration Effects 0.000 abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 abstract description 5
- 239000002250 absorbent Substances 0.000 abstract description 3
- 230000002745 absorbent Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 2
- -1 manganese oxide compound Chemical class 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 241000195493 Cryptophyta Species 0.000 abstract 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 239000011572 manganese Substances 0.000 abstract 1
- 230000010355 oscillation Effects 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 239000003403 water pollutant Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 238000011109 contamination Methods 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- 229910000616 Ferromanganese Inorganic materials 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 3
- 235000020188 drinking water Nutrition 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000014653 Carica parviflora Nutrition 0.000 description 1
- 244000132059 Carica parviflora Species 0.000 description 1
- 235000013162 Cocos nucifera Nutrition 0.000 description 1
- 244000060011 Cocos nucifera Species 0.000 description 1
- WAEMQWOKJMHJLA-UHFFFAOYSA-N Manganese(2+) Chemical compound [Mn+2] WAEMQWOKJMHJLA-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- FGIWMSAVEQNPPQ-UHFFFAOYSA-N arsenic;hydrate Chemical compound O.[As] FGIWMSAVEQNPPQ-UHFFFAOYSA-N 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002384 drinking water standard Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Water Treatment By Sorption (AREA)
Abstract
The invention supplies a new type adsorbent--mixed oxide of iron and manganese / diatomite preparation, use and regeneration method, belongs to the treatment of technology. The method used the soluble ferrous permanganate and salt as raw materials, respectively prepared the solutions, after adequate lye into permanganate solution, mixed two salt solutions, by adding diatomite particles, full oscillation, standing aging, neutralize, washing and drying to get the manganese oxide / silicon algae absorbent. The adsorbent is larger than the surface area and good adsorption properties can be used to remove arsenic in water pollutants (especially tervalence arsenic), and the adsorption surface activity of the saturated absorption of pollutants can be directly passed to load manganese oxide compound to regeneration.
Description
Technical field
The present invention relates to a kind of be used for removing water arsenic contamination thing, have a preparation method of the iron-managanese compounded oxide/diatomite adsorbant of high-specific surface area and good absorption property, the using method of this adsorbent in water treatment and the renovation process of adsorbent.The invention belongs to field of water processing technology.
Background technology
Absorption method is one of effective method of removing arsenic contamination thing in drinking water or the dirty waste water.This method is simple, is generally suitable for the water treatment system that treating capacity is big, concentration is lower.This method is an adsorbent with the insoluble solid material with high-specific surface area, superior mechanical intensity, by effect such as physical absorption, chemisorbed or ion-exchange with arsenic contamination thing sticking in the water at adsorbent surface, thereby reach the purpose of removing arsenic contamination thing in the water.
At present, the sorbing material that is used for arsenic removal has natural coral, bentonite, zeolite, red soil, cocoanut shell, coated sand, activated alumina and active carbon and natural or synthetic metal oxide and hydrous oxide thereof etc.Many sorbing materials have removal effect preferably to pentavalent arsenic (As (V)), but relatively poor to trivalent arsenic (As (III)) removal effect.Studies show that, the toxicity of As (III) is more than 60 times of As (V), and the removal of As (III) is far beyond As (V) difficulty, thus utilize oxidant that As (III) is oxidized to As (V), and then the arsenic of removing in the water by adsorption process is the common arsenic removal technology of drinking water treatment.The accessory substance that health is had potential hazard will be produced inevitably but add oxidant, so the use chemical oxidizing agent should be do not used or reduce as far as possible in the drinking water treatment process.On the other hand, in the arsenic removal material at present commonly used, material with low cost is less to the adsorption capacity of arsenic usually, and often cost is too high and have material than high-adsorption-capacity, removes applying of arsenic adsorbent material thereby limited.Therefore, research and development are with low cost and be to study both at home and abroad at present and the focus and the difficult point problem of technological development to the novel absorption material that As (III) and As (V) all have a good removal effect.
Diatomite is to have class nonmetallic mineral loose structure, cheap, has that specific area is big, absorption property is strong, light weight, characteristics such as acidproof, is widely used in filter aid, adsorbent and catalyst carrier etc.
Summary of the invention
The object of the invention:
A kind of preparation method of adsorbent-iron-managanese compounded oxide/diatomite of arsenic removal pollutant is provided, and using method and the renovation process of this adsorbent in water treatment.In the sorbing material that the present invention relates to, the diatomite with loose structure is the load matrix, and the ferrimanganic composite metal oxide is the main part for adsorbing then.The sorbing material that the present invention relates to all has the good absorption usefulness of wide spectrum to As (III) and As (V); After this material absorption is saturated, only need simple regenerative operation can recover good arsenic removal ability.
Technical scheme of the present invention:
The preparation method of iron-managanese compounded oxide/diatomite adsorbant: with permanganate and ferrous salt is raw material, be made into two kinds of solution respectively, stirring condition down adds appropriate alkaline liquor in permanganate solution, the pH scope that makes solution between 9.0-11.0, the following two kinds of salt solution mix of stirring condition; Add diatomite afterwards and shook 30-60 minutes, leave standstill, ageing 2-24 hours; The pH value of solution value is 4.0-8.0 after adding permanganate solution behind the alkali and ferrous salt reaction solution ageing; After skimming supernatant, add certain water gaging (being preferably deionized water) and clean solid and be neutralized to pH neutral, so repeat repeatedly to be neutral until water lotion with sig water or acid solution.The solid absorbent that will make by said method was warming up to 100-105 ℃ of bakings 6-24 hours afterwards again at 50-55 ℃ of following low temperature drying 1-4 hours, promptly obtained iron-managanese compounded oxide/diatomite adsorbant.
The using method of iron-managanese compounded oxide/diatomite adsorbant: the processing method based on iron-managanese compounded oxide/diatomite adsorbant removal arsenic contamination thing of the present invention is finished in absorption/regeneration integrated reactor.This reactor contains five parts such as water inlet, adsorption stuffing bed, supporting layer, delivery port, plug valve.During the normal operation of absorption, the former water that contains the arsenic contamination thing is pumped into by water inlet, with the flow velocity of the 8～12m/h adsorption stuffing bed of flowing through, can obtain good effect of removing arsenic.When iron-managanese compounded oxide/diatomite adsorbant absorption reaches capacity or handles that the arsenic contamination substrate concentration surpasses the relevant drinking water standard of country in the water, then must regenerate to adsorbent.
Iron-managanese compounded oxide/diatomite adsorbant in situ regeneration method: the delivery port of permanganate solution (add appropriate alkaline liquor and make its pH value between 9.0-11.0) from absorption/regeneration integrated reactor entered, slowly reverse flow is through packed bed, afterwards ferrous salt solution is pumped into reactor from the water inlet, make the slow positive flow of ferrous salt cross packed bed, static 2-6h after reaction finishes, be lower than 0.2mg/L with deionized water forward flushing packed column dissolubility iron concentration in water outlet, manganese ion concentration is lower than 0.1mg/L.
Characteristics of the present invention:
1. the iron-managanese compounded oxide/diatomite adsorbant preparation process is simple, with low cost.
2. iron-managanese compounded oxide/diatomite adsorbant can all show good removal effect to trivalent arsenic As (III) and pentavalent arsenic As pollutants such as (V).
3. prepared iron-managanese compounded oxide/diatomite adsorbant has that adsorption rate is fast, capacity is big, has excellent purification of water quality usefulness.
4. adopt in situ regeneration method to realize the regeneration of adsorption activity, method is simple, and regeneration effect is good.
Description of drawings
Accompanying drawing 1 and accompanying drawing 2 are respectively the structural representation of iron-managanese compounded oxide/diatomite adsorbant after iron-managanese compounded oxide/diatomite adsorbant of the present invention and the regeneration.
Reference numeral:
1. diatomite particle; 2. the ferro manganese composite oxides particle of first load; 3. the ferro manganese composite oxides particle of new load after regenerating.
Fig. 3 is absorption of the present invention/regeneration integrated reactor structural representation.
Reference numeral:
1. water inlet; 2. adsorption stuffing bed; 3. supporting layer; 4. plug valve; 5. delivery port.
Embodiment
The preparation of embodiment 1 iron-managanese compounded oxide/diatomite adsorbant: take by weighing 1.248g FeSO
47H2O and 0.237g KMnO
4, be dissolved in respectively in the 60ml water.In liquor potassic permanganate, add 2.4ml 1mol/LNaOH solution, add copperas solution then, stir fast down 60g diatomite (BET 3m
2/ g is more than 65 orders) join in the mixed liquor, continue to stir 30 minutes, leave standstill then, room temperature ageing 16 hours.Through ageing, skim supernatant, add a small amount of rare sodium hydroxide solution again and be neutralized to neutrality, add the 200ml deionized water then, stir, washed 10 minutes, filter method carries out Separation of Solid and Liquid, solid absorbent continues to add deionized water washing 3-4 time, isolate adsorbent after, be placed in the baking oven and dried by the fire 2 hours down in 50-55 ℃, be warming up to 105 ℃ and kept 8 hours, promptly get iron-managanese compounded oxide/diatomite adsorbant.
The application of embodiment 2 iron-managanese compounded oxide/diatomite adsorbants in arsenic-containing waste water is handled: the used reactor of the present invention is a glass packed column, wherein be filled with the iron and manganese oxides/diatomite adsorbant particle of preparation, the high about 0.5m of post, diameter 3.4cm, packing volume 415cm
3Certain arsenic-containing waste water, trivalent arsenic As (III) concentration 1mg/l, pH6.7.From the water inlet of packed column below, upper end water outlet, flow of inlet water 40ml/min, results of regular determination water outlet arsenic concentration.Flow through behind 170 times of packing volumes, arsenic concentration just is higher than 10 μ g/l in the water outlet.
The in-situ regeneration of embodiment 3 iron and manganese oxides/diatomite adsorbant: when arsenic concentration is higher than water quality requirement in the packed column water outlet, stop into water, in the emptying post behind the water, slowly pump into the 100ml 0.03mol/L KMnO that is added with alkali lye from the below of packed column
4Solution, from the slow copperas solution that adds 100ml 0.09mol/L in packed column top, flow velocity is 1ml/min then.Finish, water is emitted in static ageing 4 hours then, uses the deionized water rinsing packed column, and the concentration of dissolubility ferromanganese ion is lower than water quality requirement in water outlet.
The effect of removing arsenic of iron-managanese compounded oxide/diatomite adsorbant behind embodiment 4 in-situ regenerations three times: packed column is identical with example 2 with arsenic-containing waste water, trivalent arsenic As (III) concentration 1mg/l, pH6.7.From the water inlet of packed column below, upper end water outlet, flow of inlet water 40ml/min, results of regular determination water outlet arsenic concentration.Flow through behind 150 times of packing volumes, arsenic concentration just is higher than 10 μ g/l in the water outlet.
Claims (8)
1, a kind of preparation method who is used for the iron-managanese compounded oxide/diatomite adsorbant of water treatment, it is characterized in that: described iron-managanese compounded oxide/diatomite adsorbant is to be raw material with solubility permanganate and ferrous salt, be mixed with solution respectively, after in permanganate solution, adding proper quantity of lye, two kinds of salt solution mix, add granular diatomaceous earth afterwards, fully vibration; Get through ageing, neutralization, washing and dry run preparation.
2, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: the diatomite that is added is the above shot-like particles of 65 orders.
3, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: described solubility permanganate solution is sodium permanganate, liquor potassic permanganate; Ferrous salt solution is ferrous sulfate, solution of ferrous chloride.
4, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: the used alkali of the appropriate alkaline liquor of described adding is NaOH, potassium hydroxide, ammoniacal liquor, sodium carbonate, potash, add permanganate solution behind the alkali and ferrous salt reaction solution ageing after the pH value of solution value at 4.0-8.0.
5, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: in the mixed solution ferrimanganic quality than scope at 6:1 between the 3:2.
6, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: the temperature of described aging step is that room temperature, digestion time are 2-24 hours.
7, according to the described iron-managanese compounded oxide/diatomite adsorbant preparation method of claim 1, it is characterized in that: described drying steps is under 50-55 ℃ of conditions dry 1-4 hour, is warming up to afterwards 100-105 ℃ of dry 6-24 hour again.
8, according to the renovation process of the iron-managanese compounded oxide/diatomite adsorbant of the described method of claim 1 preparation, it is characterized in that: this adsorbent reactivation is by being achieved at adsorbent surface load iron manganese composite oxide again, and original position is finished in adsorption column.
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