CN101671469B - Functional material for removing nitrogen from wastewater and method of preparing same - Google Patents
Functional material for removing nitrogen from wastewater and method of preparing same Download PDFInfo
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Abstract
The invention discloses functional material for removing nitrogen from wastewater and a method of preparing the same. The functional material comprises hydrophilic resin and inorganic nano-powder which is adhered to the hydrophilic resin. The functional material is prepared by first synthesizing the hydrophilic resin, and then adding and stirring the inorganic nano-powder to the hydrophilic resin. The inorganic nano-powder accounts for 5-20 percent of the total functional material by weight. The surface of the hydrophilic resin is provided with hydrophilic groups so that the microorganisms can be adsorbed on the surface of the functional material easily and can not fall off from the surface of the functional material, and the nitrogen removing ability of the microorganisms can be kept for a long time. Because the functional material comprises the inorganic nano-powder which can increase the roughness of the surface of the functional material, the microorganisms can be steadily adsorbed on the surface of the functional material, and because the inorganic nano-powder is adhered to the hydrophilic resin, the gaps formed in the functional material is small, and accordingly the change of the stress of the functional material is slowed down when the functional material is impacted by the water flow and the breaking strength of the functional material is improved.
Description
Technical field
The present invention relates to a kind of functional material for removing nitrogen from wastewater, the invention still further relates to a kind of preparation method of this functional materials.
Background technology
China's water resources is poor relatively, and the per capita water yield is world occupancy volume per person's 25% only, and the pollution of water resources is serious day by day.An investigation according to China environmental monitoring department shows: national river water quality pollution type is an eutrophication, main nutrient pollutant is ammonia nitrogen and total nitrogen, ammonia nitrogen is mainly derived from the nitrogenous effluent and the sanitary sewage of industrial discharge in the water body, general employing microorganism carries out denitrogenation processing in waste water or the sewage disposal, the functional materials of using in the filler is as microorganism carrier, its material and manufacture craft are to the efficient of wastewater treatment process, energy consumption, stability and reliability all have a direct impact, the prior function material has a lot, as polyvinyl alcohol, polypropylene etc., but exist wetting ability poor, cause the microorganic adhesion difficulty, denitrogenation ability, and the intensity shortcoming of high easy fracture not.
Summary of the invention
An object of the present invention is to provide a kind of good hydrophilic property, be easy to make the functional materials that microorganism is adsorbed, the denitrogenation ability is strong and breaking tenacity is high.
Another object of the present invention provides each method of system of this functional materials.
For achieving the above object, the technical solution used in the present invention is: a kind of functional material for removing nitrogen from wastewater, this functional materials comprises hydrophilic resin, is bonded in the inorganic nanometer powder on the described hydrophilic resin, and the ratio that described inorganic nanometer powder accounts in described functional materials is 5%～20% (weight percent).
The raw material that forms described functional materials comprises 60%～85% solvent, 15%～30% aggregates into the resin monomer, 0.01%～0.2% initiator, 0.1%～2% chain-transfer agent, 1%～5% dispersion agent, 5%～20% inorganic nanometer powder, wherein said solvent, the described resin monomer that aggregates into, described initiator, described chain-transfer agent, described dispersion agent synthesizes described hydrophilic resin, described solvent is a methyl-sulphoxide, dimethyl formamide, a kind of or its any blended mixture in the N,N-DIMETHYLACETAMIDE, the described resin that aggregates into comprises 60%～80% the first monomers with monomer, 10%～25% the second monomer, 5%～25% 3rd monomer, described first monomer is the alkene nitrile, described second monomer is olefin acid or alkene acid esters or its mixture, described the 3rd monomer is an olefin acid sulfonate, described initiator is a kind of in Diisopropyl azodicarboxylate or the Potassium Persulphate, described chain-transfer agent is a Dodecyl Mercaptan, and described dispersion agent is a triethyl hexyl phosphoric acid, sodium laurylsulfonate, a kind of or its any blended mixture in the polyacrylamide.
Described inorganic nanometer powder is a kind of or its any blended mixture in nano imvite powder, nano diatomite powder, the nano kaoline powder.
Described alkene nitrile is vinyl cyanide, crotononitrile or its mixture.
Described second monomer is vinylformic acid, butenoic acid, methyl acrylate, ethyl propenoate, M Cr or its any blended mixture.
Described olefin acid sulfonate is vinylformic acid sodium sulfonate, vinylformic acid potassium sulfonate, methacrylic disulfonate acid or its any blended mixture.
The raw material that forms described functional materials also comprises ethylene glycol.
Described resin monomer, described initiator, described chain-transfer agent, the described dispersion agent of aggregating into of described dissolution with solvents, 50 ℃-90 ℃ and stirring velocity is to carry out polyreaction under 100r/min～600r/min, reaction times is 0.2h-2h, synthetic described hydrophilic resin, and then add described inorganic nanometer powder, stirring velocity is under 800r/min～1500r/min, and the reaction times is 6h-12h, promptly makes described functional materials.
The described functional materials that makes is placed ethylene glycol, carry out alkali reaction, make the cyan-hydrolysis on described functional materials surface become carboxyl at 150 ℃～170 ℃.
Because the present invention has adopted above technical scheme, its advantage is as follows: the surface of this hydrophilic resin has hydrophilic radical, be convenient to make microorganism absorption, and also difficult drop-off after microorganism is attached on the surface of material, make that the denitrogenation ability of microorganism is stable lasting, added inorganic nanometer powder in this functional materials, this nano-powder can increase the roughness of material surface, thereby strengthen the absorption stably of microorganism, and nano-powder is bonded on the resin, the space that makes material internal form is small, thereby has slowed down the STRESS VARIATION of material when being subjected to water impact, has increased the breaking tenacity of this material.
Embodiment
Below further set forth the present invention.
A kind of functional material for removing nitrogen from wastewater, this functional materials comprise hydrophilic resin, are bonded in the inorganic nanometer powder on the hydrophilic resin, and the ratio that inorganic nanometer powder accounts in functional materials is 5%～20% (weight percent).The surface of this hydrophilic resin has hydrophilic radical, is convenient to make microorganism absorption, and microorganism be attached on the surface of material after also difficult drop-off, thereby improved the stability of waste water treatment process.Added inorganic nanometer powder in this functional materials, this nano-powder can increase the roughness of material surface, thereby make microorganism stably to adsorb, improve the denitrogenation ability of material, and nano-powder is bonded on the resin, the space that makes material internal form is small, thereby slowed down the STRESS VARIATION of material when being subjected to water impact, thereby increased the breaking tenacity of this material, made the effective storage life of functional materials increase, reduced use cost.
Analyze the phase structure and the composition of denitrification microorganism, with the microbial molecular formula with consist of source, carry out the quantitative and composition structure determination of elementary composition, as groups of cells become water account for 80% and dry-matter account for 20%, wherein in the dry-matter organism account for 90% and inorganics account for 10%, organism is with existing microorganism molecular formula C
60H
87O
23N
12P, C
18H
19O
9N, C
11H
29O
7N and C
5H
7O
2N determines the percentage of various elements, C 45.99～54.96%, H 4.83～10.10%, O 26.78～39.02%, N 4.89～12.89% and P 2.26%, and the inorganics ratio is P 50%, S 15%, Na 11%, Ca 9%, Mg 8%, K6% and Fe 1% etc., carry out the synthetic of functional materials in the denitrogenation of waste water organic filler, determine the composition and the corresponding molecular structure of functional materials.
Select to form the raw material of functional materials, this raw material comprises 60%～85% solvent, 15%～30% aggregates into the resin monomer, 0.01%～0.2% initiator, 0.1%～2% chain-transfer agent, 1%～5% dispersion agent, 5%～20% inorganic nanometer powder, solvent wherein, aggregate into the resin monomer, initiator, chain-transfer agent, dispersion agent synthesis hydrophilic resin, solvent is a methyl-sulphoxide, dimethyl formamide, a kind of or its any blended mixture in the N,N-DIMETHYLACETAMIDE, aggregate into resin and comprise 60%～80% the first monomers with monomer, 10%～25% the second monomer, 5%～25% 3rd monomer, first monomer is the alkene nitrile, preferably, be vinyl cyanide, crotononitrile or its mixture, cyano group in the alkene nitrile provides the nitrogen element, second monomer is olefin acid or alkene acid esters or its mixture, this second monomer can be used for the wetting ability (ester group) of equilibrium function material and the ratio of carbon, preferably, be vinylformic acid, butenoic acid, methyl acrylate, ethyl propenoate, M Cr or its any blended mixture, the 3rd monomer is an olefin acid sulfonate, be used to provide element sulphur, preferably, be the vinylformic acid sodium sulfonate, the vinylformic acid potassium sulfonate, methacrylic disulfonate acid or its any blended mixture.Other elements such as phosphoric, sodium element, manganese element, potassium element, ferro element etc. provide for inorganic nanometer powder, preferably, inorganic nanometer powder is a kind of or its any blended mixture in nano imvite powder, nano diatomite powder, the nano kaoline powder.Initiator is used for the monomeric polyreaction of initiated polymerization resin, preferably, and a kind of in Diisopropyl azodicarboxylate or the Potassium Persulphate.In order not make overreact, chain-transfer agent is selected Dodecyl Mercaptan for use, dispersion agent can make nano-powder more be bonded on the resin homodisperse, and dispersion agent can be a kind of or its any blended mixture in triethyl hexyl phosphoric acid, sodium laurylsulfonate, the polyacrylamide.
When the preparation functional materials, dissolution with solvents aggregates into resin monomer, initiator, chain-transfer agent, dispersion agent, 50 ℃-90 ℃ and stirring velocity is to carry out polyreaction under 100r/min～600r/min, reaction times is 0.2h-2h, the synthesis hydrophilic resin, and then adding inorganic nanometer powder, stirring velocity is under 800r/min～1500r/min, reaction times is 6h-12h, make functional materials, this functional materials is the spinning solution that possesses certain viscosity, through spinning, be woven into specified shape, obtain finished product, can be applicable in the filler.
Specifically set forth the composition and the preparation method of functional materials below by several embodiment,
Embodiment 1:
Methyl-sulphoxide 62%
Vinyl cyanide 14%
Crotononitrile 10%
Methyl methacrylate 4%
Vinylformic acid sodium sulfonate 3%
Diisopropyl azodicarboxylate 0.05%
Dodecyl Mercaptan 0.5%
Sodium laurylsulfonate 1.45%
Polynite 6%
According to the above ratio with acrylonitrile, crotononitrile and methyl methacrylate, the vinylformic acid sodium sulfonate, dimethyl sulfoxide (DMSO), sodium laurylsulfonate joins in the reactor, and control reaction temperature adds the azobisisobutyronitrile initiated polymerization in the time of 60～70 ℃, add Dodecyl Mercaptan after 10 minutes, add the nano imvite powder after 1 hour, the repolymerization time is about 6～10h, and it is standby as spinning solution to obtain the water white transparency thick liquid.
Spinning solution packed into begins spinning in the material still of spinning-drawing machine, obtains knitting forming behind the fiber, promptly obtains finished product.
Embodiment 2:
Dimethyl formamide 60%
Crotononitrile 20%
M Cr 4%
Ethyl propenoate 3%
Methacrylic disulfonate acid 3%
Potassium Persulphate 0.05%
Dodecyl Mercaptan 0.5%
Triethyl hexyl phosphatase 11 .45%
Kaolin 8%
According to the above ratio with butylene eyeball, M Cr, ethyl propenoate, methacrylic disulfonate acid, dimethyl formamide, triethyl hexyl phosphoric acid joins in the reactor, control reaction temperature was at 60～70 o'clock, add the Potassium Persulphate initiated polymerization, add Dodecyl Mercaptan after 10 minutes, add the nano kaoline powder after 1 hour, the repolymerization time is about 10h, and it is standby as spinning solution to obtain yellow partially thick liquid.
Spinning solution packed into begins spinning in the material still of spinning-drawing machine, obtains knitting forming behind the fiber, promptly obtains finished product.
Embodiment 3:
N,N-DIMETHYLACETAMIDE 48%
Methyl-sulphoxide 10%
Vinyl cyanide 13%
Crotononitrile 10%
Butenoic acid ethyl 4%
Vinylformic acid 2%
Methacrylic disulfonate acid 4%
Diisopropyl azodicarboxylate 0.05%
Dodecyl Mercaptan 0.5%
Sodium laurylsulfonate 1.45%
Polyacrylamide 1%
Diatomite 6%
According to the above ratio with acrylonitrile, crotononitrile, butenoic acid ethyl, vinylformic acid, methacrylic disulfonate acid, N,N-DIMETHYLACETAMIDE, methyl-sulphoxide, sodium laurylsulfonate and poly-propionic acid amide etc. join in the reactor, control reaction temperature is in the time of 60～70 ℃, add the azobisisobutyronitrile initiated polymerization, add Dodecyl Mercaptan after 10 minutes, add the nano diatomite powder after 1 hour, the repolymerization time is about 10h, and it is standby as spinning solution to obtain white partially thick liquid.Spinning solution packed into begins spinning in the material still of spinning-drawing machine, obtains knitting forming behind the fiber, promptly obtains finished product.
The surface of the functional materials for preparing has sulfonic group active group and ester group, so have stronger wetting ability, if need add strongly hydrophilic, then makes spent glycol, and the raw material that promptly forms functional materials also comprises ethylene glycol.The above-mentioned functions material that makes is placed ethylene glycol, carry out alkali reaction, make the cyan-hydrolysis on functional materials surface become carboxyl at 150 ℃～170 ℃.
By analyzing the phase structure and the composition of denitrification microorganism, the functional materials of researching and developing out, use is on filler the time, structural homology based on material, microorganism is easy to be adsorbed on the filler, and has quickened the growth of microorganism at filling surface, in the Processing Test to waste water, common fillers needed 10～30 days carry out the microorganism colonization process of growth, and on this microorganism compatibility filling 7～10 day time can finish.
There are a large amount of hydrophilic radicals on this functional materials surface, and by the bonding inorganic nanometer powder increased surfaceness, be easy to make microorganism absorption, and also difficult drop-off after microorganism depends on thereon, thereby improved the efficient stable of biomembrance process waste water treatment process, made that the denitrogenation ability of microorganism is stable lasting.Furthermore, added inorganic nanometer powder in the functional materials, nano particle has slowed down the STRESS VARIATION when filler is subjected to water impact in the inner slight void that forms of filler, thereby has increased the breaking tenacity of this material, increases the service life.Moreover, functional materials also because of the existence of the high roughness on its surface and ester group and sulfonic group active group, nano-powder, also has certain adsorption to heavy metal ion.
The filler that this functional materials is made is mainly used in the biomembrance process wastewater treatment, is mainly used in the nitrogen that removes in anhydrating.During use, the suspension of filler rule is arranged, absorption, culturing micro-organisms promptly constitute the biomembrance process water technology.Also filler can be stacked, and culturing micro-organisms, handled water flows through from the filler hole, and contact filling surface microorganism, thereby the nitrogen element in the microorganism consume water are even water is purified.
For the suspension type filler, make this bionic filler divide row to hang in the water processing reactor respectively, and, it can be deposited in the reactor for chemical filler.Behind the microbial inoculant, be adsorbed on the hydrophilic active group of filling surface rapidly and in the hole, and spread growth, becoming after the maturation can be with the microbial film of filler integral coating.This culturing process approximately needs 7～10 days.After the biofilm development maturation, pollutent such as organism, nitro in the water had good removal ability.
In this filler placement and waste water, it is to sanitary sewage COD
CrClearance greater than 90%, BOD
5Clearance greater than 95%, NH
3-N (ammonia nitrogen) clearance is greater than 95%; The variation range of TN (total nitrogen) clearance is 86%～95%, and promptly the denitrification effect of this bionic high efficiency denitrogenation organic filler reaches GB18918-2002 one-level A emission standard.Use this filler with after cultivating domestication in microorganism and the trade effluent, also can handle trade effluent, as the waste water of spandex factory.COD
Cr, BOD
5Be the important overall target of evaluation water pollution degree, COD
CrThe chemical oxygen demand that adopts potassium bichromate to determine as oxygenant.BOD
5Be biological oxygen demand (BOD) on the five, refer to the be degraded amount of oxygen of post consumption of organism that the microorganism in the water can degrade.
To sum up, functional materials wetting ability of the present invention is strong, microorganism is easy in its surface attachment growth, shorten the microorganism culturing domestication time, again because in material admixture inorganic nanometer powder, when increasing the material surface roughness, also reach the strengthened effect of material internal, promptly the intensity of functional materials of the present invention and nitric efficiency are stable lasting.
Claims (7)
1. functional material for removing nitrogen from wastewater, it is characterized in that: this functional materials comprises hydrophilic resin, be bonded in the inorganic nanometer powder on the described hydrophilic resin, described hydrophilic resin is used to adsorb denitrification microorganism, the space that described inorganic nanometer powder is used to increase the surfaceness of described functional materials and makes this material internal form is small, the weight percent ratio that described inorganic nanometer powder accounts in described functional materials is 5%～20%, the raw material that forms described functional materials comprises 60%～85% solvent, 15%～30% aggregates into the resin monomer, 0.01%～0.2% initiator, 0.1%～2% chain-transfer agent, 1%～5% dispersion agent, 5%～20% inorganic nanometer powder, wherein said solvent, the described resin monomer that aggregates into, described initiator, described chain-transfer agent, described dispersion agent synthesizes described hydrophilic resin, described solvent is a methyl-sulphoxide, dimethyl formamide, a kind of or its any blended mixture in the N,N-DIMETHYLACETAMIDE, the described resin that aggregates into comprises 60%～80% the first monomers with monomer, 10%～25% the second monomer, 5%～25% 3rd monomer, described first monomer is the alkene nitrile, described second monomer is olefin acid or alkene acid esters or its mixture, described the 3rd monomer is an olefin acid sulfonate, described initiator is a kind of in Diisopropyl azodicarboxylate or the Potassium Persulphate, described chain-transfer agent is a Dodecyl Mercaptan, described dispersion agent is a triethyl hexyl phosphoric acid, sodium laurylsulfonate, a kind of or its any blended mixture in the polyacrylamide, described inorganic nanometer powder is the nano imvite powder, the nano diatomite powder, a kind of or its any blended mixture in the nano kaoline powder.
2. functional materials according to claim 1 is characterized in that: described alkene nitrile is vinyl cyanide, crotononitrile or its mixture.
3. functional materials according to claim 1 is characterized in that: described second monomer is vinylformic acid, butenoic acid, methyl acrylate, ethyl propenoate, M Cr or its any blended mixture.
4. functional materials according to claim 1 is characterized in that: described olefin acid sulfonate is vinylformic acid sodium sulfonate, vinylformic acid potassium sulfonate, methacrylic disulfonate acid or its any blended mixture.
5. functional materials according to claim 1 is characterized in that: the raw material that forms described functional materials also comprises ethylene glycol.
6. according to the preparation method of each described functional materials among the claim 1-4, it is characterized in that: described resin monomer, described initiator, described chain-transfer agent, the described dispersion agent of aggregating into of described dissolution with solvents, 50 ℃-90 ℃ and stirring velocity is to carry out polyreaction under 100r/min～600r/min, reaction times is 0.2h-2h, synthetic described hydrophilic resin, and then add described inorganic nanometer powder, stirring velocity is under 800r/min～1500r/min, reaction times is 6h-12h, promptly makes described functional materials.
7. preparation method according to claim 6 is characterized in that: the described functional materials that will make places ethylene glycol, carries out alkali reaction at 150 ℃～170 ℃, makes the cyan-hydrolysis on described functional materials surface become carboxyl.
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| CN103936155B (en) * | 2014-05-12 | 2015-08-05 | 西南大学 | A kind of method utilizing montmorillonite to improve sewage water denitrification ability |
| CN109748378A (en) * | 2017-11-06 | 2019-05-14 | 重庆干城环保科技有限公司 | A kind of production technology of making Nano surface bio-carrier |
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