CN103980517A - Modification method of suspended filler - Google Patents
Modification method of suspended filler Download PDFInfo
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- CN103980517A CN103980517A CN201410240193.8A CN201410240193A CN103980517A CN 103980517 A CN103980517 A CN 103980517A CN 201410240193 A CN201410240193 A CN 201410240193A CN 103980517 A CN103980517 A CN 103980517A
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- floating stuffing
- acid solution
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- lactic acid
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Abstract
The invention relates to a modification method of suspended filler. The modification method comprises the following steps: a, cleaning the suspended filler with deionized water, and then drying for later use; b, adding L-polylactic acid into a volatile solvent to prepare an L-polylactic acid solution of which the mass-volume ratio is 1-3%; c, adding the L polylactic acid solution prepared in the step b into sodium chloride or potassium chloride till being saturated, and then heating by a water bath till the L-polylactic acid solution is fully dissolved; d, cooling the L-polylactic acid solution treated in the step c to room temperature and then immersing the suspended filler treated in the step c in the L-polylactic acid solution and stirring; and e, removing the solvent from the surface of the suspended filler treated in the step d by a volatilization method. According to the modification method provided by the invention, active radicals are introduced to the surface of the suspended filler, so that the coarseness of the surface of the filler is increased and formation of a nitrified bio-membrane on the surface of modified filler is accelerated, thereby benefiting adherence and growth of bacteria and further enhancing the removal efficiency of NH<3>-N and TN.
Description
Technical field
The present invention relates to a kind of method of modifying of floating stuffing.
Background technology
In micro-polluted source water, contain NH
3-N (ammonia nitrogen) and TN (total nitrogen), pretreatment technology adopts biological contact oxidation process more.It in to the oxidising process of nitrogen, is the nitrification of nitrogen, be divided into nitrosification and nitrated two steps, wherein under nitrite bacteria effect, to be converted into the process of nitrite nitrogen be rate-limiting step to ammonia nitrogen, and the bacterium of being responsible for oxidation has the unfavorable features such as long and extracellular polymeric formation volume of generation cycle is low.For addressing this problem, those skilled in the art's employing forms one deck polylactic acid membrane and accelerates the processing speed to micro-Polluted Source Water on floating stuffing.But existing floating stuffing is not strong to the adhesive ability of nitrobacteria, make the biofilm formation speed on floating stuffing slower, the purifying treatment toggle speed of micro-Polluted Source Water is slowed down.
Summary of the invention
In order to solve the problem of prior art existence, the invention provides the method for modifying of a kind of floating stuffing that can strengthen floating stuffing surface biological film sticking power.
For addressing the above problem, the technical solution adopted in the present invention is as follows:
A method of modifying for floating stuffing, comprises the steps:
A. floating stuffing is cleaned up with deionized water, for subsequent use after then drying,
B. taking Poly-L-lactic acid (be called for short PLLA) as solute, join and in volatile solvent, be mixed with the Poly-L-lactic acid solution that mass volume ratio is 1-3%;
C. the Poly-L-lactic acid solution making in b step adds sodium-chlor or Repone K to saturated, then carries out heating in water bath to Poly-L-lactic acid and dissolves completely, and the temperature of described heating in water bath is 55-65 DEG C;
D. will be cooled to room temperature through the Poly-L-lactic acid solution of c step process, then by being immersed in the Poly-L-lactic acid solution of cool to room temperature through the floating stuffing of a step process and stirring Poly-L-lactic acid solution, make area load one deck Poly-L-lactic acid solution of floating stuffing;
E. utilize volatilization method to remove the solvent through the floating stuffing surface of d step process.
In the present invention, preferred scheme is that described floating stuffing is the one in polyethylene floating stuffing and polypropylene suspension filler.
In the present invention, preferred scheme is that the volatile solvent in described b step is methylene dichloride or trichloromethane.
In the present invention, preferred scheme is that the volatilization method in described e step is specially: will in stink cupboard, at least place 24 hours (herein at least comprise 24 hours, be more than or equal to 24 hours) through the floating stuffing of d step process.
Compared with prior art, advantage of the present invention is: method of modifying is easy to operation, and PLLA is biocompatible materials, toxicological harmless effect, and modifying process PLLA consumption is few, and in actual mechanical process, cost is low; After method of modifying of the present invention, floating stuffing surfaceness increases, and has increased protein adsorption quantity, is conducive to the adhesion of bacterium; Through modification, at filling surface carbonylate (C=O), carboxyl (O=C-O), hydroxyl (C-OH) active group, promote increasing of protein adsorption quantity from two angles of physical adsorption and new formation of chemical bond, the active group of filling surface can and adhere to the combination of bacterium and produce positive promoter action, accelerate the modified filler nitrated biomembranous formation in surface, more be conducive to the adhesion growth of bacterium, and then promoted NH
3the removal efficiency of-N and TN.
Below in conjunction with the drawings and the specific embodiments, the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is the filling surface pattern comparison diagram of the floating stuffing modification front and back of embodiment 1;
Fig. 2 is the filling surface chemical bond variation diagram before the floating stuffing modification of embodiment 1;
Fig. 3 is the filling surface chemical bond variation diagram after the floating stuffing modification of embodiment 1;
Fig. 4 is the filling surface protein adsorption amount comparison diagram of the floating stuffing modification front and back of embodiment 1;
Fig. 5 is that the filler of the floating stuffing modification front and back of embodiment 1 is removed NH
3-N (ammonia nitrogen) effect contrast figure.
Fig. 6 is that the filler of the floating stuffing modification front and back of embodiment 1 is removed TN (total nitrogen) effect contrast figure.
In Fig. 1, a is the floating stuffing surface tissue before modification; B is the floating stuffing surface tissue after modification; C is the floating stuffing surface microorganism upgrowth situation before modification; D is the floating stuffing surface microorganism upgrowth situation after modification.
Embodiment
Embodiment 1
A method of modifying for floating stuffing, comprises the steps:
A. floating stuffing is cleaned up with deionized water, for subsequent use after then drying, described floating stuffing is polyethylene floating stuffing;
B. with dichloromethane solvent, taking Poly-L-lactic acid as solute, be mixed with mass volume ratio and be 3% Poly-L-lactic acid solution;
C. the Poly-L-lactic acid solution making in b step adds sodium-chlor to saturated, then carries out heating in water bath to Poly-L-lactic acid and dissolves completely, and the temperature of described heating in water bath is 65 DEG C;
D. will be cooled to room temperature through the Poly-L-lactic acid solution of c step process, then by being immersed in the Poly-L-lactic acid solution of cool to room temperature through the floating stuffing of a step process and stirring Poly-L-lactic acid solution, make area load one deck Poly-L-lactic acid solution of floating stuffing;
E. by placing 24 hours through the floating stuffing of d step process, make the solvent evaporates on floating stuffing surface in stink cupboard.
Embodiment 2
A. floating stuffing is cleaned up with deionized water, for subsequent use after then drying, described floating stuffing is in polypropylene suspension filler;
B. taking trichloromethane as solvent, taking Poly-L-lactic acid as solute, be mixed with mass volume ratio and be 1% Poly-L-lactic acid solution;
C. the Poly-L-lactic acid solution making in b step adds Repone K to saturated, then carries out heating in water bath to Poly-L-lactic acid and dissolves completely, and the temperature of described heating in water bath is 58 DEG C;
D. will be cooled to room temperature through the Poly-L-lactic acid solution of c step process, then by being immersed in the Poly-L-lactic acid solution of cool to room temperature through the floating stuffing of a step process and stirring Poly-L-lactic acid solution, make area load one deck Poly-L-lactic acid solution of floating stuffing;
E. by placing 24 hours through the floating stuffing of d step process, make the solvent evaporates on floating stuffing surface in stink cupboard.
Embodiment 3
A. floating stuffing is cleaned up with deionized water, for subsequent use after then drying, described floating stuffing is polyethylene floating stuffing;
B. with methylene dichloride, taking Poly-L-lactic acid as solute, be mixed with mass volume ratio and be 2% Poly-L-lactic acid solution;
C. the Poly-L-lactic acid solution making in b step adds Repone K to saturated, then carries out heating in water bath to Poly-L-lactic acid and dissolves completely, and the temperature of described heating in water bath is 55 DEG C;
D. will be cooled to room temperature through the Poly-L-lactic acid solution of c step process, then by being immersed in the Poly-L-lactic acid solution of cool to room temperature through the floating stuffing of a step process and stirring Poly-L-lactic acid solution, make area load one deck Poly-L-lactic acid solution of floating stuffing;
E. by placing 24 hours through the floating stuffing of d step process, make the solvent evaporates on floating stuffing surface in stink cupboard.
Embodiment 4
Get the polyethylene floating stuffing adopting before modified poly ethylene floating stuffing that embodiment 1 makes and modification, then respectively its performance is detected, the performance before itself and modification is compared.
Select its surface topography of scanning electron microscope experimental observation.As shown in Figure 1, after floating stuffing modification, surfaceness increases, be gully shape, the specific surface area of filler increases (a in Fig. 1 is that the b in floating stuffing surface tissue and the Fig. 1 before modification is the floating stuffing surface tissue after modification) thereupon, thereby the growth that modified filler surface is bacterium provides more space.The reason of above result is that PLLA is carried on after filler sodium salt or sylvite gradually from its surface dissolution, and then has increased surfaceness.
After reactor start-up for some time, bacterial adhesion grows in modified suspending filler surface, bacterial classification kind presents variation than unmodified, comprise (c in Fig. 1 are the floating stuffing surface microorganism upgrowth situation after the d modification in floating stuffing surface microorganism upgrowth situation and the Fig. 1 before modification) such as tyrothricin, stock bacterium, coccuses, can find out that the floating stuffing after modification is more conducive to adhering to of microorganism and grows;
The present invention observes the chemical composition (seeing Fig. 2 and Fig. 3) of PLLA floating stuffing sample surfaces after unmodified and modification by x-ray photoelectron spectroscopy.From the spectrogram result in the region of XPS C1s, after modification, the spectrogram of filler is by unimodal to bimodal transformation, and spectrum peak shape changes obviously, illustrates that surface modification makes atomic level that variation occur.Utilize after the matching of PC swarming software, modification is at filling surface carbonylate (C=O), carboxyl (O=C-O), hydroxyl (C-OH) active group, its peak area is respectively 12.76%, 11.07% and 55.12%, the active group of filling surface can and adhere to the combination of bacterium and produce positive promoter action, thereby can help the modified filler nitrated biomembranous quick formation in surface;
As everyone knows, extracellular polymeric is mainly made up of extracellular protein and exocellular polysaccharide, and the protein adsorption ability that filling surface is higher contributes to the quick formation of extracellular polymeric and the adhesion process to filling surface thereof, thereby helps the complete three-dimensional structure of biofilm formation.As shown in Figure 4, before and after modification, filling surface is respectively 6.24 μ g/cm to the adsorptive capacity of bovine serum albumin
2with 7.31 μ g/cm
2, adsorptive capacity has increased by 17%; For being respectively 19.88 μ g/cm before and after Fibrinogen modification
2with 25.25 μ g/cm
2, protein adsorption quantity has increased by 27%.Result shows, surface modification has increased the protein adsorption quantity of filler, this is the roughness that has increased filling surface due to modification, and the active group of introducing on surface, has promoted increasing of protein adsorption quantity from two angles of physical adsorption and new formation of chemical bond;
Fig. 5 and Fig. 6 are respectively filler modified front and back NH
3the removal situation of-N, TN.As shown in Figure 5, in 32 days of reactor start-up, NH before and after modification
3the average removal rate of-N is respectively 68.06% and 71.70%, move the 24th day, its clearance reaches 71.83% and 94.17% first, the average removal rate of modified suspending filler NH3-N exceedes 78%, its average removal rate of steady operation period is greater than 90%, and result shows that modification has improved reactor start-up phase NH
3the removal effect of-N, has accelerated the start-up course of reactor.Similarly as can be seen from Figure 6, the clearance of the filling surface TN of modification is also improved, before and after modification, the average removal rate of TN is respectively 34.54% and 39.02%, average removal rate has improved 13%, result shows that surface modification not only strengthened nitrification, has promoted denitrification simultaneously.
Above-mentioned embodiment is only the preferred embodiment of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (4)
1. a method of modifying for floating stuffing, its feature comprises the steps:
A. floating stuffing is cleaned up with deionized water, for subsequent use after then drying,
B. taking Poly-L-lactic acid as solute, join and in volatile solvent, be mixed with the Poly-L-lactic acid solution that mass volume ratio is 1-3%;
C. the Poly-L-lactic acid solution making in b step adds sodium-chlor or Repone K to saturated, then carries out heating in water bath to Poly-L-lactic acid and dissolves completely, and the temperature of described heating in water bath is 55-65 DEG C;
D. will be cooled to room temperature through the Poly-L-lactic acid solution of c step process, and then will be immersed in the Poly-L-lactic acid solution of cool to room temperature through the floating stuffing of a step process and stir Poly-L-lactic acid solution;
E. utilize volatilization method to remove the solvent through the floating stuffing surface of d step process.
2. the method for modifying of floating stuffing according to claim 1, is characterized in that: described floating stuffing is the one in polyethylene floating stuffing and polypropylene suspension filler.
3. the method for modifying of floating stuffing according to claim 1, is characterized in that: the volatile solvent in described b step is methylene dichloride or trichloromethane.
4. the method for modifying of floating stuffing according to claim 1, is characterized in that the volatilization method in described e step is specially: will in stink cupboard, place at least 24 hours through the floating stuffing of d step process.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923744A (en) * | 2016-06-22 | 2016-09-07 | 哈尔滨工业大学 | Water treatment method capable of regulating and controlling rapid start of nitrification effect of biological membrane |
| CN105923744B (en) * | 2016-06-22 | 2019-07-16 | 哈尔滨工业大学 | A kind of method for treating water of regulation biomembrane nitrification quick start |
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| CN101113052A (en) * | 2007-07-13 | 2008-01-30 | 哈尔滨工业大学 | Modified suspending filler |
| US20130164802A1 (en) * | 2007-08-03 | 2013-06-27 | Robert Hickey | Moving bed biofilm reactor (mbbr) process for conversion of syngas components to liquid products |
| CN103408129A (en) * | 2013-08-19 | 2013-11-27 | 中国水产科学研究院渔业机械仪器研究所 | Degradable bio-compatible water treatment filler and preparation method thereof |
| CN103723818A (en) * | 2013-12-10 | 2014-04-16 | 郑州正佳能源环保科技有限公司 | Method for coating surface of water treatment material with polyacrylamide gel film |
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2014
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Patent Citations (4)
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| CN101113052A (en) * | 2007-07-13 | 2008-01-30 | 哈尔滨工业大学 | Modified suspending filler |
| US20130164802A1 (en) * | 2007-08-03 | 2013-06-27 | Robert Hickey | Moving bed biofilm reactor (mbbr) process for conversion of syngas components to liquid products |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923744A (en) * | 2016-06-22 | 2016-09-07 | 哈尔滨工业大学 | Water treatment method capable of regulating and controlling rapid start of nitrification effect of biological membrane |
| CN105923744B (en) * | 2016-06-22 | 2019-07-16 | 哈尔滨工业大学 | A kind of method for treating water of regulation biomembrane nitrification quick start |
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| CN103980517B (en) | 2016-05-11 |
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Effective date of registration: 20171017 Address after: 528200 Shishan Foshan hi tech Industrial Zone (Nanhai new Guicheng water works) water quality monitoring building, Guangdong, China Patentee after: Guangdong Han Zheng Detection Technology Co., Ltd. Address before: 528200 Guangdong Foshan Nanhai Nanhai Nanhai Avenue building, Guicheng Patentee before: Grandblue Environment Co., Ltd. |