CN101992068A - Nitrogen and phosphorus absorbing agent - Google Patents
Nitrogen and phosphorus absorbing agent Download PDFInfo
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- CN101992068A CN101992068A CN2009101174207A CN200910117420A CN101992068A CN 101992068 A CN101992068 A CN 101992068A CN 2009101174207 A CN2009101174207 A CN 2009101174207A CN 200910117420 A CN200910117420 A CN 200910117420A CN 101992068 A CN101992068 A CN 101992068A
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Abstract
The invention discloses a nitrogen and phosphorus absorbing agent which comprises the following raw materials in parts by mass: 100 parts of olefin monomer, 80-200 parts of attapulgite clay, 5-20 parts of auxiliary raw material, 0.05-4.0 parts of initiator and 0.05-6.0 parts of cross-linking agent. The nitrogen and phosphorus absorbing agent forms a granular product in a reaction process, is simple in preparation process and post-treatment process, has no secondary pollution, is mainly used for treating lake eutrophic water, and can also be used for purifying water bodies of life wastewater, food wastewater, animal husbandry wastewater and the like.
Description
Technical field
The present invention relates to the environmental protection water treatment field, be specifically related to a kind of nitrogen phosphorus adsorbent.
Background technology
Along with China's industrial progress and social development, water pollutes and also is on the rise, and has become the difficult problem of environmental improvement.According to environment department monitoring, national cities and towns have 100,000,000 tons of unprocessed water bodys that directly enter of sewage every day at least.Section over half water quality is polluted in the seven big water systems of the whole nation, and the water body in the whole nation 1/3 is unsuitable for fish existence, and 1/4 water body is unsuitable for irrigating, and 90% urban waters is seriously polluted, and 50% water source, cities and towns does not meet drinking water standard.Along with constant development of economy, these statistics are also continuing increasing.
Water pollutes the pollutant that is mainly produced by mankind's activity to be caused, and it comprises industrial pollution source, agricultural pollution source and domestic pollution source three parts.Characteristics such as industrial wastewater is the important pollution sources in waters, and the amount of having is big, wide, complicated component, toxicity big, be difficult for purifying, difficult.Agricultural pollution source comprises excrement of animals, agricultural chemicals, chemical fertilizer etc.China is one of the most serious country of soil erosion in the world, about 5,000,000,000 tons of annual ground surface soil number of dropouts, cause a large amount of agricultural chemicals, chemical fertilizer to flow into river, river, lake, storehouse with ground surface soil, the nitrogen of Liu Shiing, phosphorus, potassium nutrition element thereupon, make 2/3 lake be subjected to the harm of eutrophication pollution in various degree, cause algae and other biological to breed unusually, cause the variation of water transparency and dissolved oxygen, thereby cause water quality deterioration.Domestic pollution source mainly is the various washing agent that use in the urban life and sewage, rubbish, ight soil etc., mostly is nontoxic inorganic salts, and nitrogenous in the sanitary sewage, phosphorus, sulphur are many, and malignant bacteria is many.
Nitrogen and phosphorus are the main matter that causes water pollution and eutrophication as inorganic nutrient substance.Therefore, effectively remove nitrogen and phosphorus in the sewage, significant to the protection water environment.The phosphorus method of denitrogenating of report mainly contains chemical method, the precipitation method, biochemical process and absorption method both at home and abroad at present.In these methods, adsorption technology is because of having characteristics such as convenient and swift, efficient, more and more people's attention that cause.The core of adsorption technology is to select suitable sorbing material.Active carbon is the most frequently used water treatment absorbent, but it costs an arm and a leg, separation difficulty, and the regeneration condition harshness, and adsorption effect is undesirable.In recent years, utilizing molecular sieve or cheap clay that nitrogenous phosphorus waste water is carried out adsorption treatment also has report, but adsorption time is long, and adsorption capacity is low.
The compound adsorbent of organic-inorganic is new in recent years developing direction, owing in the compound adsorbent hydrophily functional groups is arranged, pollutant is had capability of fast response and high adsorbance.Introduce clay class material at compound adsorbent, can further reduce product cost.Therefore, utilize the dispersin polymerization technology,, can obtain granular attapulgite clay base composite absorbent through appropriately crosslinked processing.Such adsorbent has higher adsorption capacity and absorption/desorption rate faster to nitrogen phosphorus, has broad application prospects in high nitrogen phosphorus water undoubtedly.
Summary of the invention
The objective of the invention is to remove the limited in one's ability and desorption rate of nitrogen phosphorus and waits not enoughly slowly, provide that a kind of adsorption rate is fast, adsorption capacity big, regeneration is simple and the recyclable nitrogen phosphorus adsorbent of utilization again at general adsorbent.
The present invention realizes by following measure:
Adopt cheap attapulgite clay and the vinyl monomer key component as adsorbent, by initiated polymerization be cross-linked to form network structure, a step obtains the granular nitrogen phosphorus adsorbent.
A kind of nitrogen phosphorus adsorbent is characterized in that the mass fraction of adsorbent raw material is: 100 parts of vinyl monomers, attapulgite clay 80-200 part, auxiliary material 5-20 part, initator 0.05-4.0 part, crosslinking agent 0.05-6.0 part; Auxiliary material is an one or more combination in shitosan, humic acid, the polyvinyl alcohol; Initator is ammonium persulfate or potassium peroxydisulfate; Crosslinking agent is N, and is a kind of or two kinds in N '-methylene-bisacrylamide and the alum; The preparation method is suspended in the aqueous solution of alcohol with attapulgite clay or through the attapulgite clay that modification is handled, add auxiliary material, vinyl monomer, initator and crosslinking agent then, be warming up to 60-90 ℃ of reaction 3-5 hour, discharging, process crosslinking Treatment, dry back packing.
Vinyl monomer of the present invention is the one or more combination in acrylic acid, itaconic acid, methacrylic acid, methyl methacrylate, EMA, hydroxyethyl methacrylate, hydroxy propyl methacrylate, styrene, sulfonated phenylethylene, the dimethyl diallyl ammonium chloride.Acrylic acid, itaconic acid and methacrylic acid can with clay generation graft copolymerization, appropriateness is introduced monomers such as methyl methacrylate, EMA, hydroxyethyl methacrylate and hydroxy propyl methacrylate, helps forming granular disintegration.
The particle diameter of attapulgite clay of the present invention is below the 0.05mm, and the attapulgite clay modification can be with a kind of processing the in sulfuric acid, iron chloride, the softex kw.Attapulgite clay can further improve graft copolymerization efficient after modification is handled, form regular network structure, helps the absorption to pollutant.
Shitosan of the present invention, humic acid and polyvinyl alcohol are natural polymers, and its functional group helps strengthening absorption on the one hand, can play dispersion polymerization on the other hand, forms the partical of particle homogeneous.
In the aqueous solution of alcohol of the present invention, the mass fraction of alcohol is 5-50%.
In the aqueous solution of alcohol of the present invention, alcohol is a kind of in methyl alcohol, ethanol, isopropyl alcohol and the n-butanol.
The material that crosslinking Treatment of the present invention is used is calcium chloride or aluminium chloride.Adopt calcium chloride or aluminium chloride that product is handled, can further strengthen the intensity of particle, help repeating to re-use.
The network structure that adsorbent forms has high absorption to nitrogen phosphorus, is again simultaneously a kind of weak combination, by the dilute alkaline soln desorption, can re-use.
The present invention promptly forms granular product in course of reaction, preparation process and last handling process are simple, non-secondary pollution.This adsorbent is mainly used in the processing of lake eutrophication water, also can be used for the purified treatment of water bodys such as sanitary wastewater, food wastewater and animal husbandry waste water.
Compared with prior art, the present invention has the following advantages: 1. contain 50% above attapulgite clay in this compound adsorbent, so product cost is lower.2. this compound adsorbent swelling and not dissolving only in the nitrogen phosphorus solution can reduce the resistance to mass tranfer in the adsorbents adsorb process, makes absorption system reach adsorption equilibrium very soon, and being adsorbed on of nitrogen promptly reached balance in 3～5 min.3. under the same conditions, the adsorption capacity of this compound adsorbent be clay and active carbon 3-5 doubly.4. this compound adsorbent can use in the pH of 4-8 scope.5. this compound adsorbent can at room temperature utilize the aqueous slkali wash-out to regenerate, and possesses good serviceability repeatedly.6. adopt the TAIHU LAKE actual tests to show, be not subjected to the influence of water temperature during this compound adsorbent adsorption of nitrogen phosphorus.
The specific embodiment
The assay method of adsorption capacity of the present invention is as follows: 0.05 gram adsorbent is joined in 25mL nitrogenous (or phosphorus) solution, after the room temperature vibration 30 minutes (to phosphorus 2 hours), adopt the anti-(ammonium molybdate of nessler reagent and molybdenum antimony, potassium antimony tartrate, developer when ascorbic acid)) making nitrogen and phosphorus mensuration respectively calculates adsorption capacity according to following formula.
Wherein, Q is adsorption capacity (mg/g); C
0Be nitrogen before adsorbing or phosphorus concentration (mg/L); C
eFor adsorbing back nitrogen or phosphorus concentration (mg/L); V
0And V
eBe respectively absorption forward and backward liquor capacity (mL); M is adsorbent dry weight (mg).
Embodiment 1:
With 100 gram attapulgite clays at room temperature with after the 1000 mL 1mol/L ferric chloride solutions stirring 2 hours, add 2 gram shitosans, wait to dissolve the back and add the aqueous solution that contains itaconic acid 80 grams and acrylic acid 20 grams, the aqueous solution that adds 200 mL ethanol again, back adding N stirs, N '-methylene-bisacrylamide 0.5 gram stirs adding ammonium persulfate 0.2 gram after 30 minutes.Being warming up to 70 ℃ kept 3 hours.Carry out crosslinking Treatment with aluminium chloride after reaction is finished, packing dries to constant weight under 70 ℃ after filtering.
Embodiment 2:
With 80 gram attapulgite clays at room temperature with after the 800 mL0.1mol/L sulfuric acid solutions stirring 2 hours, add 2 gram polyvinyl alcohol, intensification is waited to dissolve the back and is added the aqueous solution that contains methacrylic acid 20 grams and acrylic acid 80 grams, the aqueous solution that adds 250 mL ethanol again, back adding N stirs, N '-methylene-bisacrylamide 1 gram stirs adding ammonium persulfate 3 grams after 30 minutes.Being warming up to 70 ℃ kept 3 hours.Carry out crosslinking Treatment with calcium chloride after reaction is finished, packing dries to constant weight under 70 ℃ after filtering.
Embodiment 3:
120 gram attapulgite clays are at room temperature restrained the stirring of softex kw solution after 2 hours with 900 mL 2.5, add 3 gram humic acid, the back adding of waiting to stir contains the aqueous solution that methyl methacrylate 10 restrains and acrylic acid 80 restrains, the aqueous solution that adds 250 mL isopropyl alcohols again, back adding N stirs, N '-methylene-bisacrylamide 2 grams stirs adding potassium peroxydisulfate 5 grams after 30 minutes.Being warming up to 70 ℃ kept 3 hours.Carry out crosslinking Treatment with calcium chloride after reaction is finished, packing dries to constant weight under 70 ℃ after filtering.
Embodiment 4:
With 120 gram attapulgite clays at room temperature with after the 900 mL running water stirring 2 hours, add 5 gram shitosans, the back adding of waiting to stir contains the aqueous solution that styrene 10 restrains and acrylic acid 80 restrains, add 250 mL methanol in water again, back adding N stirs, N '-methylene-bisacrylamide 0.5 gram stirs adding potassium peroxydisulfate 4 grams after 30 minutes.Being warming up to 70 ℃ kept 3 hours.Carry out crosslinking Treatment with calcium chloride after reaction is finished, packing dries to constant weight under 70 ℃ after filtering.
Claims (6)
1. a nitrogen phosphorus adsorbent is characterized in that the mass fraction of adsorbent raw material is: 100 parts of vinyl monomers, attapulgite clay 80-200 part, auxiliary material 5-20 part, initator 0.05-4.0 part, crosslinking agent 0.05-6.0 part; Auxiliary material is an one or more combination in shitosan, humic acid, the polyvinyl alcohol; Initator is ammonium persulfate or potassium peroxydisulfate; Crosslinking agent is N, and is a kind of or two kinds in N '-methylene-bisacrylamide and the alum; The preparation method is suspended in the aqueous solution of alcohol with attapulgite clay or through the attapulgite clay that modification is handled, add auxiliary material, vinyl monomer, initator and crosslinking agent then, be warming up to 60-90 ℃ of reaction 3-5 hour, discharging, process crosslinking Treatment, dry back packing.
2. adsorbent as claimed in claim 1 is characterized in that vinyl monomer is the one or more combination in acrylic acid, itaconic acid, methacrylic acid, methyl methacrylate, EMA, hydroxyethyl methacrylate, hydroxy propyl methacrylate, styrene, sulfonated phenylethylene, the dimethyl diallyl ammonium chloride.
3. adsorbent as claimed in claim 1, the particle diameter that it is characterized in that attapulgite clay is below the 0.05mm, the attapulgite clay modification is with a kind of processing the in sulfuric acid, iron chloride, the softex kw.
4. adsorbent as claimed in claim 1 is characterized in that in the aqueous solution of alcohol, the mass fraction of alcohol is 5-50%.
5. as claim 1 or 4 described adsorbents, it is characterized in that alcohol is for a kind of in methyl alcohol, ethanol, isopropyl alcohol and the n-butanol.
6. adsorbent as claimed in claim 1 is characterized in that the material that crosslinking Treatment is used is calcium chloride or aluminium chloride.
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| CN2009101174207A CN101992068A (en) | 2009-08-09 | 2009-08-09 | Nitrogen and phosphorus absorbing agent |
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| CN2009101174207A CN101992068A (en) | 2009-08-09 | 2009-08-09 | Nitrogen and phosphorus absorbing agent |
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Cited By (18)
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|---|---|---|---|---|
| CN103623787A (en) * | 2013-11-15 | 2014-03-12 | 西北师范大学 | Preparation method of acrylic acid/polyvinylpyrrolidone/palygorskite composite adsorbing material |
| CN105727880A (en) * | 2016-02-19 | 2016-07-06 | 甘肃工业技术研究院 | Preparing technology for environment-friendly attapulgite adsorbing/drying agent |
| CN105935587A (en) * | 2016-06-28 | 2016-09-14 | 安徽金联地矿科技有限公司 | Method using attapulgite to prepare particles for removing phosphor from water |
| CN106582546A (en) * | 2016-12-30 | 2017-04-26 | 徐州工程学院 | Plant dip dyeing liquid used for purifying nitrogen and phosphorus polluted water body and preparation method thereof |
| CN107082835A (en) * | 2016-08-21 | 2017-08-22 | 王金桢 | A kind of preparation method of Trichlorosilane purification purification aids |
| CN107159143A (en) * | 2017-06-06 | 2017-09-15 | 滁州市宏源喷涂有限公司 | A kind of preparation method of humic acid kaolin compound adsorbent for polyvinyl chloride vent gas treatment |
| CN107236071A (en) * | 2017-05-27 | 2017-10-10 | 淮阴工学院 | The preparation method and products obtained therefrom of the recessed native polystyrene resin of magnetic based on the recessed native surface modification of magnetic |
| CN107381755A (en) * | 2017-09-22 | 2017-11-24 | 苏州水木康桥环境工程技术有限公司 | A kind of environment-friendly long-life heavy metal industrial effluent inorganic agent and preparation method thereof |
| CN107413317A (en) * | 2017-08-16 | 2017-12-01 | 江苏理工学院 | Chitin modified GMA/MAA polymer absorbants and its methods and applications |
| CN107930312A (en) * | 2017-11-13 | 2018-04-20 | 陕西科技大学 | A kind of natural degradable macromolecular suppression haze spray agent and its preparation method and application |
| CN108502948A (en) * | 2018-04-23 | 2018-09-07 | 苏州清荷坊环保科技有限公司 | A kind of rural sewage filter screen |
| CN108499545A (en) * | 2018-04-02 | 2018-09-07 | 苏州清荷坊环保科技有限公司 | A kind of filter screen for adsorbing nitrogen P elements in waste water |
| CN108993451A (en) * | 2018-09-10 | 2018-12-14 | 芜湖新达园林绿化集团有限公司 | A kind of environmental protection and energy saving adsorbent and its preparation method and application |
| CN110394165A (en) * | 2019-08-12 | 2019-11-01 | 中国科学院烟台海岸带研究所 | A kind of preparation method and application of dephosphorization zeolite |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN112206748A (en) * | 2019-07-10 | 2021-01-12 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecanedioic acid |
| CN113149168A (en) * | 2021-04-27 | 2021-07-23 | 山鹰国际控股股份公司 | Water treatment composition and preparation method thereof |
| CN114452953A (en) * | 2022-01-30 | 2022-05-10 | 内蒙古大学 | Adsorbent and preparation method and application thereof |
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2009
- 2009-08-09 CN CN2009101174207A patent/CN101992068A/en active Pending
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| CN103623787A (en) * | 2013-11-15 | 2014-03-12 | 西北师范大学 | Preparation method of acrylic acid/polyvinylpyrrolidone/palygorskite composite adsorbing material |
| CN105727880A (en) * | 2016-02-19 | 2016-07-06 | 甘肃工业技术研究院 | Preparing technology for environment-friendly attapulgite adsorbing/drying agent |
| CN105935587A (en) * | 2016-06-28 | 2016-09-14 | 安徽金联地矿科技有限公司 | Method using attapulgite to prepare particles for removing phosphor from water |
| CN107082835A (en) * | 2016-08-21 | 2017-08-22 | 王金桢 | A kind of preparation method of Trichlorosilane purification purification aids |
| CN106582546A (en) * | 2016-12-30 | 2017-04-26 | 徐州工程学院 | Plant dip dyeing liquid used for purifying nitrogen and phosphorus polluted water body and preparation method thereof |
| CN107236071B (en) * | 2017-05-27 | 2019-03-26 | 淮阴工学院 | The preparation method and products obtained therefrom of the recessed soil-polystyrene resin of magnetism based on magnetic recessed native surface modification |
| CN107236071A (en) * | 2017-05-27 | 2017-10-10 | 淮阴工学院 | The preparation method and products obtained therefrom of the recessed native polystyrene resin of magnetic based on the recessed native surface modification of magnetic |
| CN107159143B (en) * | 2017-06-06 | 2020-01-17 | 滁州市宏源喷涂有限公司 | Preparation method of humic acid and kaolin composite adsorbent for polyvinyl chloride tail gas treatment |
| CN107159143A (en) * | 2017-06-06 | 2017-09-15 | 滁州市宏源喷涂有限公司 | A kind of preparation method of humic acid kaolin compound adsorbent for polyvinyl chloride vent gas treatment |
| CN107413317A (en) * | 2017-08-16 | 2017-12-01 | 江苏理工学院 | Chitin modified GMA/MAA polymer absorbants and its methods and applications |
| CN107413317B (en) * | 2017-08-16 | 2020-02-14 | 江苏理工学院 | Chitosan modified GMA/MAA polymer adsorbent and method and application thereof |
| CN107381755A (en) * | 2017-09-22 | 2017-11-24 | 苏州水木康桥环境工程技术有限公司 | A kind of environment-friendly long-life heavy metal industrial effluent inorganic agent and preparation method thereof |
| CN107930312A (en) * | 2017-11-13 | 2018-04-20 | 陕西科技大学 | A kind of natural degradable macromolecular suppression haze spray agent and its preparation method and application |
| CN108499545A (en) * | 2018-04-02 | 2018-09-07 | 苏州清荷坊环保科技有限公司 | A kind of filter screen for adsorbing nitrogen P elements in waste water |
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| CN108993451A (en) * | 2018-09-10 | 2018-12-14 | 芜湖新达园林绿化集团有限公司 | A kind of environmental protection and energy saving adsorbent and its preparation method and application |
| CN112206748A (en) * | 2019-07-10 | 2021-01-12 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecanedioic acid |
| CN112206748B (en) * | 2019-07-10 | 2023-05-26 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecade diacid |
| CN110394165A (en) * | 2019-08-12 | 2019-11-01 | 中国科学院烟台海岸带研究所 | A kind of preparation method and application of dephosphorization zeolite |
| CN111732148B (en) * | 2020-06-29 | 2022-06-10 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN111732148A (en) * | 2020-06-29 | 2020-10-02 | 河海大学 | System for retrieve phosphate in follow surface eutrophic water |
| CN113149168A (en) * | 2021-04-27 | 2021-07-23 | 山鹰国际控股股份公司 | Water treatment composition and preparation method thereof |
| CN114452953A (en) * | 2022-01-30 | 2022-05-10 | 内蒙古大学 | Adsorbent and preparation method and application thereof |
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Application publication date: 20110330 |