CN102091602A - Ammonia nitrogen adsorption material for polluted water and preparation method - Google Patents
Ammonia nitrogen adsorption material for polluted water and preparation method Download PDFInfo
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- CN102091602A CN102091602A CN2010106220740A CN201010622074A CN102091602A CN 102091602 A CN102091602 A CN 102091602A CN 2010106220740 A CN2010106220740 A CN 2010106220740A CN 201010622074 A CN201010622074 A CN 201010622074A CN 102091602 A CN102091602 A CN 102091602A
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Abstract
The invention discloses an ammonia nitrogen adsorption material for polluted water and a preparation method. The ammonia nitrogen adsorption material comprises the following components in percentage by weight: 65 to 90.5 percent of ethylene-propylene-diene monomer rubber, 9 to 34 percent of modified zeolite, and 0.5 to 1 percent of dicumyl peroxide; and the ratio of the volume mL of liquid paraffin to the total weight g of the three components is 1:100. The prepared ammonia nitrogen adsorption material for the polluted water has good adsorption rate on ammonia nitrogen in the polluted water, the adsorption capacity is increased together with the increment of the pH value at the temperature of 20 DEG C in the pH value range of between 4.0 and 6.2, and the adsorption capacity is maximum when the pH value is 6.0; and the ammonia nitrogen removal rate of the polluted water is 80 to 90 percent in the pH value range of between 4.0 and 6.2. The ammonia nitrogen adsorption value is 2.23 to 4.25mg.g<-1> at the temperature of 20 DEG C when the pH is equal to 7; and the adsorption capacity of the ammonia nitrogen adsorption material for the polluted water is 4.78mg/g at the temperature of 10 DEG C when the pH is equal to 7.
Description
Technical field
The present invention relates to inorganic mineral chemistry and adsorption science field, be specifically related to a kind of ammonia nitrogen absorption material and preparation method of polluted-water.
Background technology
Nitrogen is one of important source of students key element of natural water body, and ammonia nitrogen extensively exists in river, river, lake, sea and surface water and the underground water, is one of important indicator of water body quality evaluation.The source of ammonia nitrogen mainly contains in the water: complicated biological chemistry action takes place in the range protein organic matter in the sanitary sewage under microbial action, decomposes the NH that produces
3Industrial wastewater (as coking chemical waste water, synthetic nitrogen chemical fertilizer factory waste water etc.) and agricultural fertilizer etc.When the water body ammonia-nitrogen content is higher, very easily cause eutrophication, aquatile and people's life are caused great harm.Therefore, along with the enhancing of people's environmental protection consciousness, the technology of removing ammonia nitrogen in the former water also is the research emphasis of current water technology.
At present, the technology that is usually used in removing ammonia nitrogen in the former water mainly contains biochemical process
[1], blow-off method
[2], the break point chlorination method
[3]And absorption method
[4]Four kinds.
Biochemical process is to adopt to remove ammonia nitrogen technology more widely, comprises contact oxidation method and ozone biological activated carbon method.Contact oxidation method equipment complexity, the structures of processing are bigger, cost is big since this method influenced by water temperature very big, remove the weak effect of ammonia nitrogen during winter low temperature, the application of this technology is restricted.Ozone biological activated carbon method exists the shortcoming that investment is big, remove the ammonia nitrogen weak effect winter equally.
The operating ambient temperature of blow-off method will be more than 0 ℃, because when being lower than 0 ℃, Ammonia blowing-out tower is inoperable, and the residual dirt of calcium carbonate can deposit in the filler of stripping tower in the water simultaneously, thereby causes stripping efficient to reduce.
The break point chlorination method is water treatment plant's removal ammonia nitrogen method commonly used, but break point chlorination can increase the dosage of chlorine greatly, increases water producing cost, and the DBPs content in the water also can increase greatly, influences drinking water quality.
A kind of technology of utilizing zeolite to remove ammonia nitrogen is arranged in the absorption method.Zeolite can be divided into granular and powdery on using.Zeolite is abundant, cheap at China's reserves, adsorption capacity is big
[5], have the porosity height simultaneously, specific area is big, the performance that ion exchangeable, adsorptivity etc. are excellent
[6,7], zeolite has higher selection adsorptivity to ammonia nitrogen, therefore, utilizes zeolite to remove ammonia nitrogen and has good application prospects.
At present, the application of granular zeolite is to adopt the granular zeolite of 0.6～1.6 millimeter particle diameter to filter as filtrate and adsorb, and granular zeolite is put into related device directly use.But it is less that weak point is adsorption capacity, causes losing efficacy in the short period of time, and the regeneration period is short.Therefore, there is big problem in actual applications in granular zeolite.
If adopt the powdery zeolite to remove ammonia nitrogen, have a conspicuous contradiction: the particle diameter of zeolite is more little, and exchange capacity is higher, and is good more to pollutant removal, but the too little powder of particle diameter easily runs off with water outlet, influences effluent quality, and also can increase the loss of flood peak of operative installations.The loss of flood peak is that the unit mass water body is because of overcoming the mechanical energy that the resistance to water-flow acting is lost in the current, and the viscosity of liquid is the internal cause that produces the loss of flood peak, also is basic reason.(list of references: [1] China radiance, open ripple. contradictory relation in the municipal sewage biological dephosphorize denitrification technology and countermeasure [J]. water supply and drainage, 2000,20 (12): 2-3.[2] Xu Guoqiang, Ceng Guang is bright etc. ammonia nitrogenous wastewater treatment technology present situation and development [J]. and the Hunan non-ferrous metal, 2002,18 (2): 29-33.[3] Zhang Xiheng. water pollution control engineering [M]. Beijing: metallurgical industry publishing house, 1993,282-286.[4] Mark E.Davisand Raul F.Lobo.Zeolite and molecular sieve synthesis[J] .Chem.Mater., 1992,4 (4): 756-768.[5] Liu Yuliang, Luo Gu source etc. clinoptilolite is to the analysis of experiments [J] of ammonia nitrogen absorption performance. University Of Chongqing's journal, 2004,27 (1): 62-65.[6] MarkA.Keane.The removal of copper and nickel from aqueous solution usingY zeolite ion exchangers[J] .Colloids and Surfaces, 1998,138:11-20.[7] Hidekazu Tanaka, Norito Yamasaki, Masakazu Muratani, et al.Structureand formation process of (K, Na)-and clinoptilolite[J] .Materials ResearchBulletin 2003,38,713-722.)
Summary of the invention
The ammonia nitrogen absorption material and the preparation method that the purpose of this invention is to provide a kind of polluted-water.Raw material are modified zeolite powder, utilize organic inorganic hybridization theory and material melt blending technology to prepare a kind of compound sorbing material: this material has good absorption ammonia nitrogen ability, not only keep the cheap and good-quality characteristics of zeolite, and can effectively improve the defective that exists when adopting powdery zeolite to remove ammonia nitrogen.
The ammonia nitrogen absorption material of a kind of polluted-water provided by the invention, adopt ethylene propylene diene rubber as matrix, utilize modified zeolite after the chemical modification as filler, cumyl peroxide is as crosslinking agent, atoleine is as lubricant, utilize the method for melt blending and compression molding, directly prepare the ammonia nitrogen of the good polluted-water of a kind of absorption property and handle material.
The ammonia nitrogen absorption material of a kind of polluted-water provided by the invention, its composition and percentage by weight are as follows: the percentage by weight of ethylene propylene diene rubber, modified zeolite and cumyl peroxide is 65～90.5%: 9～34%: 0.5～1%; The volume mL number of atoleine is 1: 100 with the ratio of the gross weight g number of ethylene propylene diene rubber, modified zeolite and cumyl peroxide.
The step of the ammonia nitrogen absorption material preparation method of a kind of polluted-water provided by the invention is as follows:
(1) preliminary treatment of natural zeolite: the natural zeolite washed with de-ionized water, oven dry, grind into powder is crossed 200 eye mesh screens, obtains natural zeolite powder;
(2) with natural zeolite powder, put into the sodium chloride solution that concentration is 1mol/L, stir with the magnetic force heating stirrer, at 70 ℃ of following water-bath heating 3h, it is clean to spend deionised water, and drying obtains modified zeolite powder, and sealing is preserved standby;
(3) according to proportioning, modified zeolite powder and ethylene propylene diene rubber are mixed in the back adding Haake torque rheometer, melt temperature is 220 ℃, after mixture is molten condition, add cumyl peroxide and atoleine, put into mill again through taking out behind the melting mixing 5min, mixing temperature is 160 ℃, take out behind the 2min, obtain material just;
(4) after just material is at room temperature placed 24 hours, extrude woollenly under 160 ℃ with vulcanizing press, the dwell time is 10 minutes, woollenly behind 80 ℃ of following thermal balance 10h, obtains the ammonia nitrogen absorption material of polluted-water in vacuum drying oven.
Beneficial effect: the ammonia nitrogen absorption material of a kind of polluted-water provided by the invention, the ethylene propylene diene rubber of selecting function admirable for use is as matrix, zeolite powder after the sodium chloride modification is handled is as filler, the sorbing material of preparing possesses better adsorption capability to the ammonia nitrogen in the sewage, and obtained adsorption effect preferably in actual applications, be applicable in the bad border of water body of all kinds of ammonia and nitrogen pollutions such as neutrality and acid city and rural area, used by the canal system paddy field district of ammonia and nitrogen pollution.
The ammonia nitrogen absorption capacity of the ammonia nitrogen absorption material of a kind of polluted-water provided by the invention, when serviceability temperature remains on 20 ℃ of room temperatures, the increase with the pH value in the pH value is 2.0～6.0 scope of the adsorption capacity of the ammonia nitrogen absorption material of polluted-water increases, and is to reach maximum at 6.0 o'clock in the pH value; Increase with the pH value in the pH value is 6.0～9.0 scope reduces; In the pH value was 4.0～6.2 scopes, the ammonia nitrogen removal frank that calculates according to the adsorption capacity of the ammonia nitrogen absorption material of polluted-water was 80-90%.In the pH of environment for use value is 7 when constant, the ammonia nitrogen absorption material of polluted-water rising adsorption capacity along with temperature in 10～35 ℃ of scopes presents the trend that reduces gradually, wherein, in 10～20 ℃ of scopes, the trend that adsorption capacity reduces is very fast, when temperature be elevated to＞20 ℃ the time, the trend that the adsorption capacity adsorption capacity reduces slows down.At pH=7, temperature=20 ℃, the ammonia nitrogen absorption capacity of the ammonia nitrogen absorption material of a kind of polluted-water provided by the invention, the ammonia nitrogen absorption value is 2.23-4.25/mgg
-1PH=7, in the time of 10 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 4.78mg/g; PH=7, in the time of 20 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 4.25mg/g; PH=7, in the time of 40 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 3.17mg/g.
Description of drawings
Fig. 1 (a) is the natural zeolite powder infrared spectrogram; (b) be NaCl modified natural zeolite infrared spectrogram.
Fig. 2 (a) is a natural zeolite powder X-RD ray diagram; (b) be NaCl modified zeolite powder X-RD ray diagram.
Fig. 3 is the electron micrograph (10000 times of multiplying powers) of the ammonia nitrogen absorption material of the polluted-water that obtained by embodiment 1; (a) be the ammonia nitrogen absorption material internal deployment conditions of polluted-water; (b) be the ammonia nitrogen absorption material microstructure figure of polluted-water.
When Fig. 4 was temperature certain (20 ℃), under the different pH values, the ammonia nitrogen absorption material of polluted-water was to the comparison of ammonia nitrogen absorption clearance in the sewage.
When Fig. 5 was pH value certain (pH=7), under the different temperatures, the ammonia nitrogen absorption material of polluted-water was to the comparison of ammonia nitrogen absorption clearance in the sewage.
The specific embodiment
(1) with deionized water natural zeolite is cleaned three times, under 80 ℃ of temperature, dry, use the mortar grind into powder, cross 200 eye mesh screens, obtain 200 order natural zeolite powders.
(2) get 200 order natural zeolite powders, put into the sodium chloride solution of 1mol/L, the magnetic force heating stirrer stirs, and at 70 ℃ of following water-bath heating 3h, it is clean to spend deionised water, and drying obtains modified zeolite powder, and sealing is preserved standby.
(3) modified zeolite powder and ethylene propylene diene rubber are mixed, mixture is added in the Haake torque rheometer, melt temperature is 220 ℃, after mixture is molten condition, add cumyl peroxide (DCP), the weight ratio of ethylene propylene diene rubber, modified zeolite powder and cumyl peroxide is 65%: 34%: 1%; Drip the 1mL atoleine.Directly put into mill through taking out behind the melting mixing 5min, mixing temperature is 160 ℃, takes out behind the shearing processing 2min and obtains material just.
(4) after just material was at room temperature placed 24 hours, extruding diameter with vulcanizing press under 160 ℃ was the circular woollen of 1mm for 75mm thickness, and the dwell time is 10 minutes.Woollen in vacuum drying oven, behind 80 ℃ of following thermal balance 10h, obtain the ammonia nitrogen absorption material of polluted-water, be designated as A
1
The weight ratio of ethylene propylene diene rubber, modified zeolite powder and cumyl peroxide is 90.5%: 9%: 0.5%; Step (2) at 70 ℃ of following water-baths heating 3h, remaining obtains the ammonia nitrogen absorption material of polluted-water with embodiment 1, is designated as A
2
Embodiment 3
The weight ratio of ethylene propylene diene rubber, modified zeolite powder and cumyl peroxide is 75%: 24.3%: 0.7%;
Step (2) at 70 ℃ of following water-baths heating 3h, remaining obtains the ammonia nitrogen absorption material of polluted-water with embodiment 1, is designated as A
3
The ammonia nitrogen absorption capacity of the ammonia nitrogen absorption material of table 1 a kind of polluted-water provided by the invention
| Production code member | Ammonia nitrogen absorption value/mgg -1 |
| A 1 | 4.25 |
| A 2 | 2.23 |
| A 3 | 3.86 |
Annotate: the test condition of table 1: pH=7, temperature=20 ℃.
Adopt infra-red sepectrometry to characterize through the zeolite powder before and after the sodium chloride modification, as shown in Figure 1.The characteristic absorption peak of natural zeolite is 122620cm
-1, 1082.29cm
-1, 800.45cm
-1, 545.40cm
-1The skeletal vibration frequency of zeolite molecules changes and changes along with silica alumina ratio.Infrared curve can be found out in the comparison diagram, and resulting zeolite of modification and natural zeolite are at 1000cm
-1(antisymmetric stretching vibration of sial tetrahedron) and 420cm
-1～500cm
-1(silicon oxygen bond flexural vibrations) have characteristic absorption peak, and this illustrates both framework type bone basically identicals.But the characteristic absorption peak of modified zeolite is lower than natural zeolite.This molar fraction that can infer aluminium in the skeleton increases, and just silica alumina ratio reduces.This be because the adhesion of A1-O key than the Si-O key a little less than, its valency electric constant is also inevitable less, this deducibility bond distance's increase or electronegativity reduce, and cause that the force constant of key reduces, thereby vibration frequency is reduced, adsorption capacity strengthens.
Before and after the sodium chloride modification X-RD ray spectrogram of zeolite powder as shown in Figure 2, obvious variation has taken place in the feature of the X-RD of modified zeolite powder spectrum, the one, spectrum shape, the 2nd, the intensity of diffracted ray.Modified zeolite powder is compared with zeolite powder, d increases relatively in the PERFORMANCE OF MODIFIED VERMICULITE sample, and the partial spectrum peak disappears, reason may be the sodium chloride corrosion, decomposed the organic or inorganic impurity in the zeolite pores, dredged the duct, owing to vermiculite wafer breakage under the effect of interlayer solvent, present the porous feature simultaneously, the wafer pitch of zeolite is increased.
The ammonia nitrogen absorption material of polluted-water is by its microstructure of electron microscope observation, as shown in Figure 3.Fig. 3 (a) is the ammonia nitrogen absorption dispersion of materials photo of polluted-water, is uniformly dispersed, and aggregation phenomenon do not occur, and matrix surface is flawless.The ammonia nitrogen absorption material surface of polluted-water is cellular among Fig. 3 (b), and specific area is big, so advantages of good adsorption effect.
Product A
1～A
3To the ammonia nitrogen absorption capacity of ammonia nitrogen simulated wastewater (measure environmental condition: pH=7, temperature=20 ℃), as shown in table 1.Show the increase of product, to the adsorption capacity increase of ammonia nitrogen in the simulated wastewater along with the modified zeolite powder addition.
The present invention is keeping environment for use temperature-resistant, during 20 ℃ of room temperatures, in the pH of broad value scope (pH=2.0～9.0), the ammonia nitrogen absorption materials A of polluted-water has been discussed
1To the absorption of ammonia nitrogen, the pH value is one of principal element of influence absorption.H with 1mol/L
2SO
4And the NaOH of 2mol/L regulates the pH value of sewage, configuration pH value be 2.0,3.0,4.0,5.0,6.0,7.0,8.0,9.0 contain ammonia nitrogen simulated wastewater 100mL, the ammonia nitrogen initial concentration is 50mg/L, puts into 250mL ground tool plug triangular flask respectively, and each adds the sorbing material A of 5g
1, it contains the amount of ammonia nitrogen to filter mensuration after the adsorption equilibrium, and calculates clearance.
As shown in Figure 4, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water increases with the pH value in 2.0～6.0 scopes, is to reach maximum at 6.0 o'clock in the pH value; Then, the increase with the pH value reduces in the pH value is 6.0～9.0 scopes; In the pH value was 4.0～6.2 scopes, the ammonia nitrogen removal frank that calculates according to the adsorption capacity of the ammonia nitrogen absorption material of polluted-water was 80-90%.
Embodiment 5
Get 2g sorbing material A respectively
1Being added to mass concentration is in the ammonia nitrogen simulated wastewater of 50mg/L, and the pH value is 7, neutrality.Place the 5h that vibrates on the constant temperature oscillator, pH value of aqueous solution is 7.3, and the bath temperature interval is 10～35 ℃, calculates the pH value and be 7 when constant, A under the condition of different temperatures
1Adsorption capacity.
As shown in Figure 5, remained on 7 o'clock in the pH of environment for use value, temperature has very big influence to the adsorption capacity of the ammonia nitrogen absorption material of polluted-water, along with the rising adsorption capacity of temperature presents the trend that reduces gradually, as in 10～20 ℃ of lower temperature ranges, with the rising of temperature, the trend that adsorption capacity is decrescence little is very fast, when temperature be elevated to＞20 ℃ the time, the trend that adsorption capacity is decrescence little slows down.In the time of 10 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 4.78mg/g, and in the time of 20 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 4.25mg/g, and in the time of 40 ℃, the adsorption capacity of the ammonia nitrogen absorption material of polluted-water is 3.17mg/g.
Claims (4)
1. polluted-water ammonia nitrogen absorption material, its composition and percentage by weight are as follows: the percentage by weight of ethylene propylene diene rubber, modified zeolite and cumyl peroxide is 65～90.5%: 9～34%: 0.5～1%; The volume mL number of atoleine is 1: 100 with the ratio of the gross weight g number of ethylene propylene diene rubber, modified zeolite and cumyl peroxide.
2. a kind of polluted-water ammonia nitrogen absorption material as claimed in claim 1, it is characterized in that its composition and percentage by weight are as follows: the percentage by weight of ethylene propylene diene rubber, modified zeolite and cumyl peroxide is 65%: 34%: 1%.
3. a kind of polluted-water ammonia nitrogen absorption material as claimed in claim 1, it is characterized in that its composition and percentage by weight are as follows: the percentage by weight of ethylene propylene diene rubber, modified zeolite and cumyl peroxide is 90.5%: 9%: 0.5%.
4. a kind of polluted-water ammonia nitrogen absorption material as claimed in claim 1, the step of its preparation method is as follows:
(1) preliminary treatment of natural zeolite: the natural zeolite washed with de-ionized water, oven dry, grind into powder is crossed 200 eye mesh screens, obtains natural zeolite powder;
(2) with natural zeolite powder, put into the sodium chloride solution that concentration is 1mol/L, stir with the magnetic force heating stirrer, at 70 ℃ of following water-bath heating 3h, it is clean to spend deionised water, and drying obtains modified zeolite powder, and sealing is preserved standby;
(3) according to proportioning, modified zeolite powder and ethylene propylene diene rubber are mixed in the back adding Haake torque rheometer, melt temperature is 220 ℃, after mixture is molten condition, add cumyl peroxide and atoleine, put into mill again through taking out behind the melting mixing 5min, mixing temperature is 160 ℃, take out behind the 2min, obtain material just;
(4) after just material is at room temperature placed 24 hours, extrude woollenly under 160 ℃ with vulcanizing press, the dwell time is 10 minutes, woollenly behind 80 ℃ of following thermal balance 10h, obtains polluted-water ammonia nitrogen absorption material in vacuum drying oven.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105749884A (en) * | 2016-03-28 | 2016-07-13 | 柳州联海科技有限公司 | Nitrogen-ammonia adsorbent prepared from modified chestnut shells and production method |
| CN106430873A (en) * | 2016-11-01 | 2017-02-22 | 中国海洋大学 | High-efficiency compound type substrate improver and preparation method |
| CN108212086A (en) * | 2018-01-19 | 2018-06-29 | 北京师范大学 | For the modified activated carbon absorbent and its preparation process of Adsorption ammonia nitrogen |
| CN108928875A (en) * | 2018-07-20 | 2018-12-04 | 张莉敏 | A kind of dedicated improver of water quality in fish pond and preparation method thereof |
-
2010
- 2010-12-30 CN CN2010106220740A patent/CN102091602A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105749884A (en) * | 2016-03-28 | 2016-07-13 | 柳州联海科技有限公司 | Nitrogen-ammonia adsorbent prepared from modified chestnut shells and production method |
| CN106430873A (en) * | 2016-11-01 | 2017-02-22 | 中国海洋大学 | High-efficiency compound type substrate improver and preparation method |
| CN108212086A (en) * | 2018-01-19 | 2018-06-29 | 北京师范大学 | For the modified activated carbon absorbent and its preparation process of Adsorption ammonia nitrogen |
| CN108928875A (en) * | 2018-07-20 | 2018-12-04 | 张莉敏 | A kind of dedicated improver of water quality in fish pond and preparation method thereof |
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Application publication date: 20110615 |