CN104492404A - Granular adsorbent as well as preparation method and application of granular adsorbent in adsorption of ammonia nitrogen - Google Patents
Granular adsorbent as well as preparation method and application of granular adsorbent in adsorption of ammonia nitrogen Download PDFInfo
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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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
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a granular adsorbent as well as a preparation method and application of the granular adsorbent in adsorption of ammonia nitrogen. The granular adsorbent comprises the following components in parts by weight: 3-5 parts of a framework material, 3-4 parts of an adhesive, 1-3 parts of a pore-forming agent and 1-2 parts of functional substances, wherein the framework material is Kanuma soil or Akadama soil; the binder is bentonite, natural zeolite powder or montmorillonite; the pore-forming agent is corn starch, soluble starch, polyvinylpyrrolidone or urea; and the functional substances are sodium chloride, sodium sulfate or sodium nitrate. The preparation method comprises the following steps of uniformly mixing the components to obtain a mixture, adding deionized water into the mixture, blending into paste, molding, drying and sintering for a sintering time of 1-2 hours at 400-800 DEG C. The granular adsorbent has the advantages of wide sources, low cost, high adsorption performance to ammonia nitrogen in high-concentration ammonia nitrogen wastewater, no need of further treatment and no secondary pollution to the environment.
Description
Technical field
The invention belongs to sorbing material synthesis and application, more particularly, relate to granule adsorbent of ammonia nitrogen and preparation method thereof in a kind of removal waste water synthesized by differed clay mineral.
Background technology
In recent years, along with the fast development of industry, the industries such as rare earth, chemical industry, iron and steel create a large amount of high-concentration ammonia nitrogenous wastewaters, if not treated direct discharge, the oxidation of ammonia nitrogen can cause dissolved oxygen concentration in water body to reduce, and cause quality of river water to turn black smelly, water quality is seriously deteriorated.Meanwhile, in water, the too high meeting of nitrogen content causes algae sharply to increase, and causes the eutrophication of water body.Under favourable environmental condition, ammonia nitrogen can change into nitrite nitrogen, nitrate nitrogen further, the water drinking azotate pollution can cause serious harm to health, nitrate can be poisonous nitrite by micro-reduction in human body, ferrous iron in hemoglobin can be converted into ferric iron by nitrite, make red blood cell sex change, hemoglobin no longer has oxygen carrying capacity, causes human body to occur phenomenon of suffocating.Baby's Acidity in the stomach, lower than adult, is conducive to the growth of nitrate reduction bacterium, so baby is more more responsive than adult to the genotoxic potential of nitrate, makes baby easily suffer from methemoglobinemia." GB8978-2002 integrated wastewater discharge standard " primary standard regulation ammonia nitrogen of China's implementation from 1 day January in 1998 must not more than 15mg/L, and secondary standard regulation ammonia nitrogen must not more than 25mg/L (medical raw material, dyestuff, petrochemical enterprise must not more than 50mg/L).
Treatment technology at present to nitrogen-containing wastewater, mainly contains physical chemistry and the large class of biologic treating technique two.Employed physico-chemical techniques comprises break point chlorination method, chemical precipitation method, ion-exchange, blow-off method, hyperfiltration etc., and the usual service condition of these methods is strict, causes cost higher due to a large amount of chemical agent of needs or the energy.Microbial method is removed ammonia nitrogen and is comprised nitrated, denitrification two processes, common bio-denitrification technology mainly contains activated sludge process and biomembrance process, although cost is lower, the anti-HI high impact load-bearing capacity of microorganism is poor, is unsuitable for the process of high-concentration ammonia nitrogenous wastewater.Ammonia nitrogen in absorption method absorption waste water is safe and reliable and cost is lower, and adsorbent common at present mainly contains bentonite, zeolite, CNT, flyash, active carbon etc.The usual particle of these adsorbents is tiny, specific surface large, high adsorption capacity, has higher ion-exchange performance.In existing Study and appliance, the adsorbent such as zeolite, active carbon has the variforms such as Powdered, graininess usually, but the adsorption by soil agent such as bentonite mostly are Powdered.These powdered adsorbents is difficult to Separation of Solid and Liquid, not free settling, and granular adsorbent treatment process is fairly simple, consumption of power is few, is easy to recycling.Because natural adsorbent exists its limitation in the application; the existing much research be optimized for above-mentioned adsorbent; such as; in the granulating research of adsorption by soil agent; existing research is raw material with sodium bentonite, stirring evenly through adding water after mixing appropriate amount of starch, coal dust or mud, extruding, dry, high-temperature roasting, obtained porous bentonite clay particle after cooling.But current most adsorbent elements is comparatively single, its modification technology to environment, and normally may process for low concentration ammonia nitrogen waste water, to the ammonia nitrogen absorption poor effect in high-concentration ammonia nitrogenous wastewater.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of granule adsorbent and preparation method thereof is provided, wide material sources, with low cost, for the ammonia nitrogen absorption function admirable in high-concentration ammonia nitrogenous wastewater, without the need to subsequent treatment, secondary pollution is not caused to environment.
Technical purpose of the present invention is achieved by following technical proposals:
Granule adsorbent, composed of the following components according to parts by weight: framework material 3-5 parts, binding agent 3-4 parts, pore-foaming agent 1-3 parts, functional materials 1-2 parts, wherein:
Described framework material is deer natural pond soil or red beautiful soil, or the mixture that deer natural pond is native and red beautiful soil mixes with 1:1 mass ratio;
Described binding agent is bentonite, natural zeolite powder or imvite;
Described pore-foaming agent is cornstarch, soluble starch, polyvinylpyrrolidone (PVP) or urea;
Described functional materials is sodium chloride, sodium sulphate or sodium nitrate.
In technique scheme, the parts by weight of each component are preferably as follows: framework material 3.5-5 parts, binding agent 3-3.5 parts, pore-foaming agent 1-2.5 parts, functional materials 1-1.5 parts.
In technique scheme, the Particle size requirements of each component is: framework material is 80-105 μm; Binding agent is 50-100 μm; Pore-foaming agent is 10-40 μm; Functional materials is 100-200 μm.
The preparation method of above-mentioned granule adsorbent, carries out according to following step:
Framework material, binding agent, pore-foaming agent and functional materials is taken according to described mass fraction and Particle size requirements, after mixing, add deionized water wherein and be modulated into pasty state aftershaping, sinter at 400-800 DEG C after drying to be formed, sintering time is 1-2h.
In technique scheme, be shaped to shape, sheet or graininess, be advisable with spherical particle, particle diameter remains on 2 – 3mm.
In technique scheme, baking temperature is selected to be 90-110 DEG C of drying 20-24h.
In technique scheme, sintering temperature is 550-600 DEG C, and sintering time is 1.5-2h.
The application of above-mentioned granule adsorbent in absorption ammonia nitrogen, utilize granule adsorbent of the present invention to adsorb ammonia nitrogen in water body, ammonia nitrogen absorption action principle is ion-exchange:
Wherein M is the electronegative functional group in clay mineral surface.This adsorbent provides Na by sodium salt
+, with NH
4 +carry out ion-exchange, thus remove the ammonia nitrogen in waste water.The adsorption reaction equilibration time of adsorbent of the present invention can reach 480min, to NH
4 +(theory) adsorption capacity of-N can reach 112.4mgg
-1.This adsorbent take salic minerals as main chemical compositions, and comprise sodium salt provides Na simultaneously
+as NH
4 +exchange ion, to NH
4 +-N has selective compared with macroion, when there is cation in waste water solution as Na
+, K
+, Ca
2+, Mg
2+time, adsorbent still has higher ammonia nitrogen absorption removal effect.
Adsorb aperture distributional analysis according to BJH, the hole aperture of the adsorbent more than 65% in the present invention is 2-50nm, BET specific surface area 36-37m
2g
-1; Langmuir specific area is 33-35m
2g
-1; T-plot specific area is 40-42m
2g
-1; Total pore space amount is 0.10-0.15cm
3g
-1.
Compared with prior art, feature of the present invention is: the raw material of synthetic adsorbent is natural minerals, wide material sources, with low cost; Adsorbent is large for the advantages of good adsorption effect of high-concentration ammonia nitrogenous wastewater, adsorption capacity; Adsorbent removal ammonia nitrogen in the present invention is the principle based on ion-exchange, the generation of no coupling product; Adsorbent after absorption can be used as nitrogenous fertilizer, can improve soil property, the ability that improve the slow-release capability of nitrogenous fertilizer and the maintenance nutrient of soil used in combination with traditional nitrogenous fertilizer, and environmental sound; Adsorbent in the present invention is without the need to after-treatment.Present invention reduces the processing cost of ammonia nitrogen waste water, thus improve the practicality that absorption method removes ammonia nitrogen in high-concentration ammonia nitrogenous wastewater.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below in conjunction with specific embodiment.The deer natural pond soil (SiO that following embodiment uses
2: 56.20%, Al
2o
3: 38.70%, Fe
2o
3: 2.20%, CaO:2.00%, MgO:0.36%) and red beautiful soil (SiO
2: 51.30%, Al
2o
3: 38.05%, Fe
2o
3: 7.67%, MgO:1.94%, CaO:0.78%, MnO:0.26%) purchased from Makino Store, Kiyosu, Japan, the deer natural pond soil of selection 80-105 μm of sieving respectively and red beautiful soil (powder).Binding agent bentonite, natural zeolite powder, imvite, purchased from Azuwan Cement Factory, Japan, select 50-100 μm of powders after sieving.Pore-foaming agent (cornstarch, soluble starch, polyvinylpyrrolidone, urea) and functional materials (sodium chloride, sodium sulphate, sodium nitrate) are purchased from Wako Pure Chemical Industries.Ltd, Japan, selects the powder of 10-40 μm and the powder of 100-200 μm after sieving respectively.
Embodiment 1
Native for red jade 2g, deer natural pond soil 2g, natural zeolite powder 3g, soluble starch 2.5g, sodium sulphate 1g are fully mixed, add deionized water and be modulated into pasty state, manually be shaped to the spherical particle of particle diameter 2 – 3mm, with 105 DEG C of dry 24h, 600 DEG C of sintering 1.5h in Muffle furnace, be cooled to room temperature, be directly stored in plastics PE bottle, sealing, constant temperature are preserved.
Embodiment 2
Native for red jade 5g, imvite 3.5g, cornstarch 3g, sodium nitrate 1.5g are fully mixed, add deionized water and be modulated into pasty state, manually be shaped to the spherical particle of particle diameter 2 – 3mm, with 90 DEG C of dry 20h, 400 DEG C of sintering 2h in Muffle furnace, be cooled to room temperature, be directly stored in plastics PE bottle, sealing, constant temperature are preserved.
Embodiment 3
Deer natural pond soil 5g, bentonite 4g, urea 1g, sodium chloride 2g are fully mixed, add deionized water and be modulated into pasty state, manually be shaped to the spherical particle of particle diameter 2 – 3mm, with 110 DEG C of dry 24h, 550 DEG C of sintering 1.5h in Muffle furnace, be cooled to room temperature, be directly stored in plastics PE bottle, sealing, constant temperature are preserved.
Embodiment 4
Deer natural pond soil 3g, natural zeolite powder 4g, polyvinylpyrrolidone 2.5g, sodium sulphate 2g are fully mixed, add deionized water and be modulated into pasty state, manually be shaped to the spherical particle of particle diameter 2 – 3mm, with 100 DEG C of dry 24h, 800 DEG C of sintering 1h in Muffle furnace, be cooled to room temperature, be directly stored in plastics PE bottle, sealing, constant temperature are preserved.
Following prevailing quality detection is carried out to adsorbent of the present invention:
1. specific area and BJH (Barrett-Joyner-Halenda) pore-size distribution
Measured by Brunauer-Emmett-Teller (BET) surface analysis instrument (Coulter SA3100, US).In BJH analyzes, apply absorption and analytic technique mensuration pore area and specific pore volume amass.
2. ammonia nitrogen absorption experiment
Carry out in 50mL sealed plastic pipe under room temperature (25 ± 3 DEG C), manually prepare NH
4cl solution (2500-10000mgL
-1), all by NH
4cl is dissolved in deionized water and prepares.Adsorbent amount is 5 to 40gL
-1, be immersed in by adsorbent in ammonia nitrogen solution, adsorbance increases with the increase of adsorption time and reaches stable gradually, and adsorption time is 8h.In addition, by NaCl, KCl, MgCl
2, CaCl
2concentration is provided to be 200mgL respectively
-1competitiveness to coexist cation Na
+, K
+, Mg
2+, Ca
2+, be 5000mgL in ammonia nitrogen solution concentration
-1, adsorbent amount is 20gL
-1condition under measure competitive cationic impact.Ammonia nitrogen concentration is measured by ammonia nitrogen instrument (ION METER TiN-9001, Japan).
Work as NH
4cl solution concentration is 5000mgL
-1time, the ammonia nitrogen absorption effect of each embodiment is as following table:
The ammonia nitrogen absorption effect of each embodiment of table 1
By in table shown in data, sintering temperature, sintering time are too high or too low, and the ammonia nitrogen absorption effect of adsorbent all can be made to reduce.Meanwhile, different framework materials and the adsorption effect of the selection of functional materials to adsorbent have a significant effect.For embodiment 1, ammonia nitrogen absorption effect can reach more than 20%, illustrate that adsorbent of the present invention has reasonable application prospect in high-concentration ammonia nitrogenous wastewater absorption, adopt same procedure to test adsorbent prepared by all the other embodiments and all show identical character.
Adsorption experiment condition on the impact of ammonia nitrogen absorption effect as following table.
Table 2 uses the different N H of embodiment 1
4the ammonia nitrogen absorption effect of Cl solution
Table 3 uses the ammonia nitrogen absorption effect of the different adsorbent amount of embodiment 1
Ammonia nitrogen absorption effect when table 4 uses the competitive cation of the difference of embodiment 1 to coexist
Experimental result shows, to high concentration NH
4cl solution is (as 10000mgL
-1), when haydite adsorbent amount is 20gL
-1, when time of contact is 8h, the maximum ammonia nitrogen removal frank of adsorbent, higher than 15%, is deposited in case at coexisting ion, and adsorbent still maintains higher NH
4 +ion selectivity.Illustrate that this adsorbent can reach the Expected Results of absorption ammonia nitrogen completely, and be convenient to store and transport.
To the specific area of primary granule thing and this adsorbent and void content measurement result as following table:
Table 5 specific area and void content
Adsorb aperture distributional analysis according to BJH, the hole aperture of the adsorbent more than 65% in the present invention is 2-50nm.Analyze according to BJH pore-size distribution, the main chemical compositions of the adsorbent in the present invention is salic minerals, and comprise sodium salt provides Na simultaneously
+as NH
4 +exchange ion.
Above to invention has been exemplary description; should be noted that; when not departing from core of the present invention, any simple distortion, amendment or other those skilled in the art can not spend the equivalent replacement of creative work all to fall into protection scope of the present invention.
Claims (8)
1. granule adsorbent, is characterized in that, the hole aperture of described adsorbent more than 65% is 2-50nm, BET specific surface area 36-37m
2g
-1; Langmuir specific area is 33-35m
2g
-1; T-plot specific area is 40-42m
2g
-1; Total pore space amount is 0.10-0.15cm
3g
-1composed of the following components according to parts by weight: framework material 3-5 parts, binding agent 3-4 parts, pore-foaming agent 1-3 parts, functional materials 1-2 parts, take framework material, binding agent, pore-foaming agent and functional materials, after mixing, add deionized water wherein and be modulated into pasty state aftershaping, sinter at 400-800 DEG C after drying to be formed, sintering time is 1-2h, wherein:
Described framework material is deer natural pond soil or red beautiful soil, or the mixture that deer natural pond is native and red beautiful soil mixes with 1:1 mass ratio; Described binding agent is bentonite, natural zeolite powder or imvite; Described pore-foaming agent is cornstarch, soluble starch, polyvinylpyrrolidone or urea; Described functional materials is sodium chloride, sodium sulphate or sodium nitrate.
2. granule adsorbent according to claim 1, is characterized in that, the parts by weight of each component are preferably as follows: framework material 3.5-5 parts, binding agent 3-3.5 parts, pore-foaming agent 1-2.5 parts, functional materials 1-1.5 parts.
3. granule adsorbent according to claim 1, is characterized in that, the Particle size requirements of each component is: framework material is 80-105 μm; Binding agent is 50-100 μm; Pore-foaming agent is 10-40 μm; Functional materials is 100-200 μm.
4. the preparation method of granule adsorbent, is characterized in that, carries out according to following step:
Framework material, binding agent, pore-foaming agent and functional materials is taken according to described mass fraction and Particle size requirements, after mixing, add deionized water wherein and be modulated into pasty state aftershaping, sinter at 400-800 DEG C after drying to be formed, sintering time is 1-2h, wherein:
Framework material 3-5 parts, binding agent 3-4 parts, pore-foaming agent 1-3 parts, functional materials 1-2 parts, described framework material is deer natural pond soil or red beautiful soil, or the mixture that deer natural pond is native and red beautiful soil mixes with 1:1 mass ratio; Described binding agent is bentonite, natural zeolite powder or imvite; Described pore-foaming agent is cornstarch, soluble starch, polyvinylpyrrolidone or urea; Described functional materials is sodium chloride, sodium sulphate or sodium nitrate; Framework material is 80-105 μm; Binding agent is 50-100 μm; Pore-foaming agent is 10-40 μm; Functional materials is 100-200 μm.
5. the preparation method of granule adsorbent according to claim 4, is characterized in that, is shaped to shape, sheet or graininess, is advisable with spherical particle, and particle diameter remains on 2 – 3mm.
6. the preparation method of granule adsorbent according to claim 4, is characterized in that, selects baking temperature to be 90-110 DEG C of drying 20-24h.
7. the preparation method of granule adsorbent according to claim 4, is characterized in that, described sintering temperature is 550-600 DEG C, and sintering time is 1.5-2h.
8. the application of the granule adsorbent as described in one of claim 1-3 in absorption ammonia nitrogen, it is characterized in that, described adsorbent provides Na
+as NH
4 +exchange ion, to NH
4 +the adsorption capacity of-N can reach 112.4mgg
-1.
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| CN106902749A (en) * | 2017-03-30 | 2017-06-30 | 山东智普信息科技有限公司 | A kind of water quality detection material and its preparation method and application |
| CN108178451A (en) * | 2016-04-06 | 2018-06-19 | 金华知产婺源信息技术有限公司 | The processing system of ammonia nitrogen in a kind of removal sanitary wastewater |
| CN110282784A (en) * | 2019-07-26 | 2019-09-27 | 合肥九一化工科技有限公司 | A kind of laboratory waste liquid processing method |
| CN111054304A (en) * | 2019-12-25 | 2020-04-24 | 中国计量大学 | Method for modifying natural zeolite by sodium nitrate combined roasting, product and application thereof |
| CN111360047A (en) * | 2018-12-25 | 2020-07-03 | 四川农业大学 | Application of red jade soil, method for removing phosphorus in farmland ditch and plant cultivation medium |
| CN111701578A (en) * | 2020-06-30 | 2020-09-25 | 广西夏阳环保科技有限公司 | Adsorbent for sewage treatment and preparation method thereof |
| CN114100596A (en) * | 2020-08-28 | 2022-03-01 | 中国石油化工股份有限公司 | Alpha-alumina carrier and preparation method thereof, silver catalyst and method for producing ethylene oxide by ethylene epoxidation |
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| CN108178451B (en) * | 2016-04-06 | 2021-05-07 | 江西清绿环保有限公司 | Treatment system for removing ammonia nitrogen in domestic wastewater |
| CN106902749A (en) * | 2017-03-30 | 2017-06-30 | 山东智普信息科技有限公司 | A kind of water quality detection material and its preparation method and application |
| CN106902749B (en) * | 2017-03-30 | 2019-06-14 | 山东智普信息科技有限公司 | A kind of water quality detection material and its preparation method and application |
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| CN111054304B (en) * | 2019-12-25 | 2022-11-01 | 中国计量大学 | Method for modifying natural zeolite by sodium nitrate combined roasting, product and application thereof |
| CN111701578A (en) * | 2020-06-30 | 2020-09-25 | 广西夏阳环保科技有限公司 | Adsorbent for sewage treatment and preparation method thereof |
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