CN102600796B - Denitrification filter material for absorbing ammonia and nitrogen and regenerating method thereof - Google Patents
Denitrification filter material for absorbing ammonia and nitrogen and regenerating method thereof Download PDFInfo
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- CN102600796B CN102600796B CN201210089218.XA CN201210089218A CN102600796B CN 102600796 B CN102600796 B CN 102600796B CN 201210089218 A CN201210089218 A CN 201210089218A CN 102600796 B CN102600796 B CN 102600796B
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Abstract
The invention discloses denitrification filter material for absorbing ammonia and nitrogen and a regenerating method of the denitrification filter material. The filter material comprises the following raw materials: 20-35% of activated aluminum oxide, 15-30% of magnesium carbonate, 25-30% of ball clay, 8-15% of potassium carbonate, 2-6% of sodium chloride, 2-6% of iron oxide and 3-8% of silicon oxide. The denitrification filter material is formed by mixing and roasting various natural mineral powder and metallic oxide, is high in using efficiency, convenient and low in cost, and solves the problems that the filter material can not be utilized repeatedly for a long time and the regenerating process of the filter material is complicated in the prior art.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of denitrogenation filtrate and renovation process thereof that adsorbs ammonia nitrogen.
Background technology
As the important composition element of organic life entity, there is a cyclic process in nitrogen in natural environment.Due to urban population, concentrate relative with municipal sewage treatment ability unfavorablely, and agricultural production used chemical fertilizer in a large number, makes the ammonia nitrogen in surface water body reach higher concentration.2007,132.4 ten thousand tons of ammonia nitrogen discharge capacitys (not containing agricultural sources) in the waste water of the environmental statistics whole nation.Wherein, 34.1 ten thousand tons of industrial ammonia nitrogen discharge capacitys, account for 26% of ammonia nitrogen total emission volumn.98.3 ten thousand tons of urban life ammonia nitrogen discharge capacitys, account for the more than 74% of ammonia nitrogen total emission volumn.China's ammonia nitrogen discharge capacity is greatly the main reason that causes current surface water body ammonia nitrogen to exceed standard far beyond environmental carrying capacity, the pollutional load pressure of receiving water body.Ammonia nitrogen has surpassed COD becomes the primary index that affects surface water quality of water environment, and country's " 12 " ammonia nitrogen total emission volumn requires to control 10%.So the processing of ammonia nitrogen in water has been become to the important research contents in one, China's water pollution control field.
For a long time, municipal sewage two stage treatment is mainly with COD
crbe to remove target with SS, not good to the removal effect of the inorganic nutrient substances such as ammonia nitrogen, and the regeneration of secondary effluent from sewage treatment plant is the important channel of saving water resource, therefore, effectively in control and reduction water, the content of ammonia nitrogen has become a urgent problem, and how to adopt inexpensive, practical low-concentration ammonia-nitrogen treatment technology, is one of current research emphasis.At present, the method for denitrogenation of waste water mainly contains chemical method, coagulant sedimentation, biochemical process and absorption method both at home and abroad.Chemical method and Coagulation with Treatment effect stability, ammonia nitrogen removal frank is high, and easy and simple to handle, yet produce be difficult in a large number salt in the mud processed and water outlet the drawbacks limit such as concentration increase applying of it; Biochemical rule requires higher on controlling and managing, and is difficult for maintaining high and stable denitrification effect; Absorption method the advantage such as can reuse with efficiently quick, simple to operate, non-secondary pollution, the adsorbent of its uniqueness and more and more cause people's concern.Conventional sorbing material mainly contains active carbon, activated alumina, silica gel, zeolite and synthetic zeolite etc. both at home and abroad.But these sorbing materials have, poor stability, adsorption capacity are low, the shortcoming such as frequent of regenerating.
Summary of the invention
Technical problem to be solved by this invention is for the problem of denitrogenation material absorption ammonia nitrogen weak effect and regeneration technology complexity in prior art, and a kind of denitrogenation filtrate and renovation process thereof that adsorbs ammonia nitrogen is provided.The method has the ammonia nitrogen that displacement goes out the absorption of denitrogenation filtrate, thereby makes denitrogenation filtrate have advantages of Reusability for a long time.
The object of the invention is to realize in the following manner:
A kind of absorption ammonia nitrogen denitrogenation filtrate, this filtrate comprises the raw material components of following percentage by weight: activated alumina 20～35%, magnesium carbonate 15～30%, ball clay 25～30%, potash 8～15%, sodium chloride 2～6%, iron oxide 2～6%, silica 3～8%.Each component sum is 100%.
The raw material components of this filtrate preferably includes: activated alumina 20～30%, magnesium carbonate 15～25%, ball clay 25～28%, potash 8～12%, sodium chloride 3～6%, iron oxide 2～5%, silica 5～8%.Each component sum is 100%.
The raw material components of this filtrate most preferably comprises: activated alumina 25～30%, magnesium carbonate 15～20%, ball clay 25～26%, potash 9～11%, sodium chloride 4～6%, iron oxide 2～4%, silica 6～8%.Each component sum is 100%.
The particle size range of ball clay of the present invention is 60～100 microns.
The preparation method of above-mentioned denitrogenation filtrate comprises the following steps:
After each raw material is mixed, add composite mineralizer, again this mixture speed with 8～10 ℃/min in oxygen atmosphere is heated up, be warming up to 650～750 ℃ and keep reaction 0.5～1.5 hour, continue to be warming up to 900～1000 ℃ and keep 0.5～1.5 hour, 1050～1200 ℃ keep 0.5～1.5 hour, 1250～1300 ℃ keep 20～40 minutes, finally be warming up to 1320～1350 ℃ and place 0.5～1 hour, washing, described composite mineralizer is by BaCO
3with TiO
2mix and form, weight ratio is 2～2.5: 3, and composite mineralizer addition is 1.5～4% of raw material gross weight.Product of the present invention can produce the microcellular structure that is greater than 50%.
The renovation process of above-mentioned denitrogenation filtrate comprises the following steps:
The sodium-salt aqueous solution that is 2～10% by mass concentration by denitrogenation filtrate dipping, floods 1.0～6.0 hours, preferably 1.0～2.0 hours, the denitrogenation filtrate having flooded is taken out.Sodium salt used is at least one in sodium chloride, sodium sulphate or sodium acetate, and the concentration of described sodium-salt aqueous solution is preferably 5～8%, and the part by weight of sodium-salt aqueous solution and denitrogenation filtrate can be 3～8: 1.
Renovation process of the present invention has adopted shorter dip time, and at normal temperature dipping, has prevented that in dipping process, denitrogenation filter structure destroys.Burn till after washing, can wash away surperficial aluminium, active site is fully exposed, increase the activity of denitrogenation filtrate.NH in solution
4 +energy of adsorption on sodium type denitrogenation filtrate meets Vermeulen model, its coefficient R=0.98, diffusion coefficient D=1.86 * 10 well
-10m
2.S
-1.Owing to mending sodium in regenerative process, make the denitrogenation filtrate sodium atom after regeneration enter denitrogenation filtrate skeleton, this has increased the heat endurance of denitrogenation filtrate.
Adopt denitrogenation filtrate of the present invention to can be used for processing high ammonia-nitrogen wastewater.
The invention has the beneficial effects as follows: denitrogenation filtrate of the present invention mainly adopts multiple natural ore powder and metal oxide mixed-forming, pass through uniform temperature, the novel filtrate of Regularization meticulously sintering into, particle diameter of filter medium can be between 5～8mm, internal voids is large, and absorption specific surface area is large, and ammonia nitrogen in water content is had to good adsorption effect, treatment conditions are neutral, and ammonia nitrogen saturated extent of adsorption of the present invention can be up to 10mg/g.
For operating characteristics and the long as far as possible life-span of obtaining, denitrogenation filtrate must regeneration after using certain hour.Adopt filtrate after the inventive method regeneration with fresh, the decay of its absorption property and mechanical performance and aging be low-down, denitrogenation filtrate of the present invention saturated extent of adsorption after using 3 years reduces only 10～15%, and under the same terms, natural zeolite is used after 3 years without absorption and power of regeneration.It is efficient, convenient, with low cost that denitrogenation filtrate of the present invention is used, and solved the problem that in prior art, filtrate can not be recycled for a long time and regeneration technology is comparatively complicated.
Accompanying drawing explanation
Fig. 1 is the sodium salt concentration relationship figure of ammonia nitrogen concentration and regenerated liquid in regenerated liquid.
The specific embodiment
By specific embodiment, further illustrate the present invention below.But the detail of embodiment only, for explaining the present invention, should not be construed as limited overall technical solution.
Embodiment 1
The raw material of denitrogenation filtrate forms (percentage by weight): activated alumina 30%, magnesium carbonate 20%, 80 microns of ball clays 25%, potash 10%, sodium chloride 5%, iron oxide 3%, silica 7%.
The preparation method of denitrogenation filtrate: after each raw material is mixed, add composite mineralizer, again this mixture speed with 10 ℃/min in oxygen atmosphere is warming up to 700 ℃ of maintenance reactions 1 hour, 1000 ℃ keep 1 hour, 1100 ℃ keep 1 hour, and 1250 ℃ keep 30 minutes, are finally warming up to 1320 ℃ of placements and within 1 hour, carry out natural packing, this filtrate produces the microcellular structure that is greater than 50%, and the filtrate after natural packing is carried out to 2 washings; Wherein, composite mineralizer is BaCO
3with TiO
2mix and form, weight ratio is 2: 3, and composite mineralizer addition is 2.6% of above-mentioned raw materials gross weight.
Denitrogenation filtrate is processed ammonia nitrogen waste water (water inlet NH
4 +concentration is 50mg/L): in the lucite post that is 10cm at diameter, pack denitrogenation filtrate 4kg into, the nitrogen-containing wastewater that concentration is 50mg/L passes through lucite post with the flow of 2L/h, measures its water outlet ammonia nitrogen concentration.Result shows: temperature is 25 ℃, and pH is neutral, and flow velocity is under 2L/h condition, single-stage denitrogenation filtrate treatment effeciency (water outlet NH
4 +concentration < 15mg/L) be 40L/kg, when saturated, treating capacity is 160L/kg; When with 3 lucite post series operations, the denitrogenation filtrate of 12kg can be removed NH altogether
4 +concentration is that about ammonia nitrogen waste water 772L of 50mg/L is to discharge standard (water outlet NH
4 +concentration < 15mg/L).
The raw material of denitrogenation filtrate forms (percentage by weight): activated alumina 20%, magnesium carbonate 21%, 100 microns of ball clays 28%, potash 12%, sodium chloride 6%, iron oxide 5%, silica 8%.
The preparation method of denitrogenation filtrate: after each raw material is mixed, add composite mineralizer, again this mixture speed with 10 ℃/min in oxygen atmosphere is warming up to 700 ℃ of maintenance reactions 1 hour, 1000 ℃ keep 1 hour, 1100 ℃ keep 1 hour, and 1250 ℃ keep 30 minutes, are finally warming up to 1320 ℃ of placements and within 1 hour, carry out natural packing, this filtrate produces the microcellular structure that is greater than 50%, and the filtrate after natural packing is carried out to 2 washings; Wherein, composite mineralizer is BaCO
3with TiO
2mix and form, weight ratio is 2: 3, and composite mineralizer addition is 1.5% of above-mentioned raw materials gross weight.
Denitrogenation filtrate is processed ammonia nitrogen waste water (water inlet NH
4 +concentration is 50mg/L): in the lucite post that is 10cm at diameter, pack denitrogenation filtrate 4kg into, the nitrogen-containing wastewater that concentration is 50mg/L passes through lucite post with the flow of 2L/h, measures its water outlet ammonia nitrogen concentration.Result shows: temperature is 25 ℃, and pH is neutral, and flow velocity is under 2L/h condition, single-stage denitrogenation filtrate treatment effeciency (water outlet NH
4 +concentration < 15mg/L) be 40L/kg, when saturated, treating capacity is 160L/kg; When with 3 lucite post series operations, the denitrogenation filtrate of 12kg can be removed NH altogether
4 +concentration is that about ammonia nitrogen waste water 770L of 50mg/L is to discharge standard (water outlet NH
4 +concentration < 15mg/L).
Embodiment 3
The raw material of denitrogenation filtrate forms (percentage by weight): activated alumina 15%, magnesium carbonate 30%, 100 microns of ball clays 25%, potash 15%, sodium chloride 3%, iron oxide 6%, silica 6%.
The preparation method of denitrogenation filtrate: after each raw material is mixed, add composite mineralizer, again this mixture speed with 8 ℃/min in oxygen atmosphere is warming up to 650 ℃ of maintenance reactions 1 hour, 950 ℃ keep 1 hour, 1200 ℃ keep 1 hour, and 1300 ℃ keep 20 minutes, are finally warming up to 1350 ℃ of placements and within 1 hour, carry out natural packing, this filtrate produces the microcellular structure that is greater than 50%, and the filtrate after natural packing is carried out to 2 washings; Wherein, composite mineralizer is BaCO
3with TiO
2mix and form, weight ratio is 2.5: 3, and composite mineralizer addition is 4% of above-mentioned raw materials gross weight.
Denitrogenation filtrate is processed ammonia nitrogen waste water (water inlet NH
4 +concentration is 50mg/L): in the lucite post that is 10cm at diameter, pack denitrogenation filtrate 4kg into, the nitrogen-containing wastewater that concentration is 50mg/L passes through lucite post with the flow of 2L/h, measures its water outlet ammonia nitrogen concentration.Result shows: temperature is 25 ℃, and pH is neutral, and flow velocity is under 2L/h condition, single-stage denitrogenation filtrate treatment effeciency (water outlet NH
4 +concentration < 15mg/L) be 40L/kg, when saturated, treating capacity is 160L/kg; When with 3 lucite post series operations, the denitrogenation filtrate of 12kg can be removed NH altogether
4 +concentration is that about ammonia nitrogen waste water 768L of 50mg/L is to discharge standard (water outlet NH
4 +concentration < 15mg/L).
Embodiment 4
NaCl regeneration denitrogenation filtrate:
Get 100g and adsorbed saturated denitrogenation filtrate (ammonia nitrogen saturated extent of adsorption is 10mg/g), being placed in mass concentration and being 5.85% the NaCl aqueous solution floods, NaCl solution use amount is 0.685L, after standing 1h, the denitrogenation filtrate having flooded is taken out, and 90～110 ℃ dry.Measure NH in regenerated liquid (NaCl solution)
4 +-N concentration.Result shows: it is 1450mg/L that the filtrate preparing according to embodiment 1 method obtains ammonia nitrogen concentration in regenerated liquid through regeneration, in the regenerated liquid that the filtrate preparing according to embodiment 2 methods obtains through regeneration, ammonia nitrogen concentration is 1445mg/L, and in the regenerated liquid that the filtrate preparing according to embodiment 3 methods obtains through regeneration, ammonia nitrogen concentration is 1439mg/L.
Embodiment 5
Na
2sO
4regeneration denitrogenation filtrate:
Get 100g and adsorbed saturated denitrogenation filtrate (ammonia nitrogen saturated extent of adsorption is 10mg/g), be placed in mass concentration and be 7.1% Na
2sO
4in the aqueous solution, flood Na
2sO
4solution use amount is 0.58L, after standing 2h, the denitrogenation filtrate having flooded is taken out, and 90～110 ℃ dry.Measure regenerated liquid (Na
2sO
4solution) NH in
4 +-N concentration, result shows: in the regenerated liquid that the filtrate preparing according to embodiment 1 method obtains through regeneration, ammonia nitrogen concentration is 1710mg/L, in the regenerated liquid that the filtrate preparing according to embodiment 2 methods obtains through regeneration, ammonia nitrogen concentration is 1700mg/L, and in the regenerated liquid that the filtrate preparing according to embodiment 3 methods obtains through regeneration, ammonia nitrogen concentration is 1691mg/L.
Embodiment 6
Get 100g and adsorbed saturated denitrogenation filtrate (ammonia nitrogen saturated extent of adsorption is 10mg/g), add the Na of variable concentrations gradient
2sO
4solution, measures NH after standing 6h respectively
4 +-N, Na
2sO
4solution use amount is respectively 0.6L.Na
2sO
4when solution concentration is increased to 10% from 2%, in regenerated liquid, ammonia nitrogen concentration is increased to 1655mg/L by 760mg/L, and ammonia nitrogen eluting rate increases thereupon, but works as Na
2sO
4when concentration of polymer solution is increased to 8%, ammonia nitrogen eluting rate tends towards stability, and considers cost and solubility, and the concentration of solution is preferably 5～8%, and most preferably 6～8%.
Claims (9)
1. a denitrogenation filtrate that adsorbs ammonia nitrogen, is characterized in that this filtrate comprises following raw material components: activated alumina 20～
35%, magnesium carbonate 15～30%, ball clay 25～30%, potash 8～15%, sodium chloride 2～6%, iron oxide 2～6%, silica 3～8%; Its preparation method is: after each raw material is mixed, add composite mineralizer, again this mixture speed with 8～10 ℃/min in oxygen atmosphere is heated up, be warming up to 650～750 ℃ and keep reaction 0.5～1.5 hour, continuing to be warming up to 900～1000 ℃ keeps 0.5～1.5 hour, 1050～1200 ℃ keep 0.5～1.5 hour, and 1250～1300 ℃ keep 20～40 minutes, are finally warming up to 1320～1350 ℃ and place 0.5～1 hour after washing; Described composite mineralizer is by BaCO
3with TiO
2mix and form, weight ratio is 2～2.5:3, and composite mineralizer addition is 1.5～4% of raw material gross weight.
2. denitrogenation filtrate according to claim 1, is characterized in that this filtrate comprises following raw material components: active oxygen
Change aluminium 20～30%, magnesium carbonate 15～25%, ball clay 25～28%, potash 8～12%, sodium chloride 3～6%, iron oxide 2～5%, silica 5～8%.
3. denitrogenation filtrate according to claim 1, is characterized in that this filtrate comprises following raw material components: active oxygen
Change aluminium 25～30%, magnesium carbonate 15～20%, ball clay 25～26%, potash 9～11%, sodium chloride 4～6%, iron oxide 2～4%, silica 6～8%.
4. according to the denitrogenation filtrate described in claim 1,2 or 3, it is characterized in that the particle size range of described ball clay is 60～100 microns.
5. a preparation method for denitrogenation filtrate claimed in claim 1, is characterized in that the method comprises the following steps:
After each raw material is mixed, add composite mineralizer, again this mixture speed with 8～10 ℃/min in oxygen atmosphere is heated up, be warming up to 650～750 ℃ and keep reaction 0.5～1.5 hour, continuing to be warming up to 900～1000 ℃ keeps 0.5～1.5 hour, 1050～1200 ℃ keep 0.5～1.5 hour, and 1250～1300 ℃ keep 20～40 minutes, are finally warming up to 1320～1350 ℃ and place 0.5～1 hour after washing; Described composite mineralizer is by BaCO
3with TiO
2mix and form, weight ratio is 2～2.5:3, and composite mineralizer addition is 1.5～4% of raw material gross weight.
6. the renovation process of the denitrogenation filtrate described in the arbitrary claim of claim 1～4, is characterized in that the method comprises the following steps:
The sodium-salt aqueous solution that is 2～10% by mass concentration by denitrogenation filtrate dipping, floods 1.0～6.0 hours, and the denitrogenation filtrate having flooded is taken out.
7. the renovation process of denitrogenation filtrate according to claim 6, is characterized in that sodium salt used is at least one in sodium chloride, sodium sulphate or sodium acetate.
8. the renovation process of denitrogenation filtrate according to claim 6, is characterized in that the concentration of described sodium-salt aqueous solution is 5～8%.
9. the renovation process of denitrogenation filtrate according to claim 6, the part by weight that it is characterized in that sodium-salt aqueous solution and denitrogenation filtrate is 3～8:1.
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| CN104341027B (en) * | 2013-07-25 | 2016-12-28 | 常州市排水管理处 | A kind of efficient decolorizing dephosphorization filler and preparation method and decolouring phosphorus removing method |
| CN105293829A (en) * | 2015-11-17 | 2016-02-03 | 昆明理工大学 | Method for filtering livestock and poultry breeding wastewater by utilizing bagasse |
| CN105582896B (en) * | 2016-01-07 | 2018-03-27 | 曹胜伟 | A kind of novel ammonia nitrogen wastewater treatment material and preparation method thereof |
| CN105906164A (en) * | 2016-06-23 | 2016-08-31 | 陈朝民 | Method for removing ammonia nitrogen in waste water |
| CN110935422B (en) * | 2019-12-18 | 2022-03-29 | 华能山东发电有限公司 | Process for enriching heavy metals in desulfurization wastewater based on high-stability adsorbent |
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