CN105268410A - Preparation method and use method of antibiotic adsorption film - Google Patents
Preparation method and use method of antibiotic adsorption film Download PDFInfo
- Publication number
- CN105268410A CN105268410A CN201510855579.4A CN201510855579A CN105268410A CN 105268410 A CN105268410 A CN 105268410A CN 201510855579 A CN201510855579 A CN 201510855579A CN 105268410 A CN105268410 A CN 105268410A
- Authority
- CN
- China
- Prior art keywords
- solution
- antibiotic
- culture dish
- film
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of an antibiotic adsorption film, and belongs to the technical field of preparation of organic-inorganic composite films. The preparation method comprises the following steps: 1, dissolving soluble chitosan into a glacial acetic acid aqueous solution, and recording as a solution A; 2, dissolving lanthanum nitrate into water, preparing into a solution, and recording as a solution B; 3, mixing a certain amount of the solution A and a certain amount of the solution B, adding glycerinum, stirring, and recording as a solution C; 4, putting the solution C into a culture dish, uniformly spreading the solution C, putting the culture dish into a drying box for drying, and preparing a dried composite film; and 5, separating the dried composite film from the culture dish, and preparing the antibiotic adsorption film. The invention further discloses a use method of the antibiotic adsorption film. The use method comprises the steps of feeding the antibiotic adsorption film into antibiotic-containing wastewater, and stirring. The antibiotic adsorption film prepared by the preparation method is low in cost, simple to prepare, high in degrading rate and convenient to use, and is particularly suitable for treatment on antibiotic type medicine wastewater.
Description
Technical field
The present invention is specifically related to a kind of preparation method and using method of antibiotic adsorbed film, belongs to Organic inorganic film preparing technical field.
Background technology
Antibiotic is the large class of one in antimicrobial agents, is the biological chemical substance produced in metabolic process; After antibiotic usage, most is discharged with ight soil with medicine original shape usually; antibiotic content in sewage treatment plant's Inlet and outlet water is very high; basin water body is caused to pollute by antibiotic; in scale livestock farming animal wastes, antibiotic concentration is also very high, antibioticly in plant to use and discharge is one of antibiotic important sources in ground surface environment.Although antibiotic is discharged in soil, water and air, can redistribute, antibiotic easily adsorbs and is accumulated in soil and water environment, damages it.Therefore the antibiotic residue eliminated in water environment all has important Research Significance to guarantee Water resources security and human survival.
Based on the serious harm that antibiotic causes the mankind, the antibiotic physical method of process mainly contains absorption, coagulation, membrane separating method at present.Membrane separation technique mainly utilizes the selection separation function of film, realizes being separated of antibiotic molecule and hydrone, membrane separation technique have efficient, energy-conservation, simple to operate, be suitable for the advantages such as strong.
Shitosan is called chitosan poly glucosamine, extensively be present in occurring in nature, in the shellfish shells such as such as shrimp crab or in the cell membrane of rudimentary plant, it is the organic resource that the earth extensively exists, Viscosity of Chitosan is large, good film-forming property, has very strong adsorptivity, fine to the treatment effect of medicine waste water.Rare earth element has extremely strong chemism, and it is wide that Rare Earth Lanthanum exists the high and purposes of content in Rare Earth Mine, is widely used in Adsorbent modification research in water treatment.At present, have a lot about shitosan as the technology of medicine waste water flocculant, ubiquity flocculating effect is poor, the problems such as adsorption efficiency is low, complicated operation.The present invention mainly replaces flocculant with shitosan-rare earth composite membrane, and by the antibiotic in film and the abundant Contact-sorption waste water of waste water, after being taken out by film, this antibiotic is by absorption degradation, avoids the complex process that waste water is separated with flocculant.
Summary of the invention
Therefore, the object of the invention is to provide a kind of with low cost, and preparation is simple, and degradation rate is high, the preparation method of antibiotic adsorbed film easy to use, and described preparation method comprises the following steps:
Soluble chitosan is dissolved in the glacial acetic acid aqueous solution by step one, is designated as solution A;
Step 2 is water-soluble by lanthanum nitrate, wiring solution-forming, is designated as solution B;
Step 3 gets a certain amount of solution A and solution B mixing, adds glycerine and stirs, being designated as solution C;
Solution C is placed in culture dish by step 4, sprawls evenly, culture dish is put into drying box dry, makes dry composite film;
Dry composite film is separated with culture dish by step 5, makes antibiotic adsorbed film.
Further, described step one is specially and is dissolved in the glacial acetic acid aqueous solution of configure 2% by soluble chitosan, and magnetic agitation is dissolved completely to Chitosan powder, is designated as solution A.
Further, described step 3 is specially gets a certain amount of solution A and solution B mixing, and wherein solution A quality mA is 10:1≤mA:mB≤10:3 with the ratio of the quality mB of solution B, add glycerine, magnetic agitation 24 hours, is designated as solution C, solution C is placed in ultrasonic cleaning machine, vibration 30min.
Further, described step 4 is specially and solution C is placed in culture dish, and wherein the volume V of solution C is 3.5mL≤V≤5mL, culture dish uses 6cm glass culture dish, sprawls evenly, culture dish is put into electric drying oven with forced convection, 60 DEG C of dryings 12 hours, make dry composite film.
Further, described step 5 is specially and is separated with culture dish by dry composite film, and separation method is the NaOH solution immersion with 2%, dry composite film is separated with culture dish, makes antibiotic adsorbed film.
Present invention also offers a kind of using method of antibiotic adsorbed film, described using method is in the antibiotic adsorbed film input antibiotic waste water made by said method and stirs.
Further, in described using method with antibiotic adsorbed film first with distilled water flushing to neutral, dry under room temperature, then to drop in antibiotic waste water and magnetic agitation.
Shitosan itself has antibacterial effect, more effective than general bacteriostatic agent and nontoxic, and rare earth ion is also found to have the pharmacological actions such as anticancer, sterilization.Shitosan plays adsorption bridging effect in water treatment and effect caught by net, and rare earth ion serves absorption charge neutrality effect and compression double electric layer effect, and the two cooperatively interacts and can play better adsorption effect.
Beneficial effect of the present invention is: in the preparation method of a kind of antibiotic adsorbed film of the present invention and using method, and shitosan wide material sources are cheap, economical and practical.Rare Earth Lanthanum is rich reserves in Rare Earth Mine, and output is large, and with the lanthanum nitrate of composite membrane, purity requirement is low, is easy to obtained.Both mixing can be good at administering medicine waste water, and degradation rate is high.The present invention, mainly for the process of residual antibiotic in medicine waste water, after wastewater treatment, only needs film to take out, does not need to be separated with flocculant, simple to operate, can meet the requirement of environmental protection.The present invention is particularly useful for the process of antibiotics waste water.
Accompanying drawing explanation
Fig. 1 be XRF in the specific embodiment of the invention 1 wastewater treatment before and after test result comparison diagram.
Detailed description of the invention
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described:
The soluble chitosan used in following detailed description of the invention, also referred to as water soluble chitosan, refers to the shitosan that energy is water-soluble.
Detailed description of the invention 1
1, accurately measure glacial acetic acid 20ml in 1000ml volumetric flask, adding distil water constant volume, dose volume mark be 2% acetum for subsequent use.
2, get 0.5g Chitosan powder and be placed in 100ml beaker, add the acetum of 20ml2%, dissolve completely to shitosan by magnetic agitation, the transparent shape of solution, wiring solution-forming A.
3, get 0.05g lanthanum nitrate and be placed in 100ml beaker, add 20ml distilled water, lanthanum nitrate is dissolved completely, wiring solution-forming B.
4, solution A and B are blended in the beaker of another 100ml, add 0.8g glycerine, magnetic agitation 24h.Now the mass ratio of shitosan and lanthanum nitrate is 10:1, and qualities of glycerin concentration is 2%, and liquor capacity is 40ml, and the volume adding glycerine is ignored, and is designated as solution C.
5, C is placed in ultrasonic cleaning machine, sonic oscillation 30min, removes bubble.
6, accurately measure solution C, 3.5ml is in the glass culture dish of 6mm in diameter, sprawls evenly.
7, the culture dish completing film is placed in electric drying oven with forced convection, keeps 60 DEG C of dryings 12 hours, final obtained dry composite film.
8, prepare the NaOH solution that 1000ml mass concentration is 2%, add 20ml in culture dish, soak, until film separates with culture dish.
9, again by film distilled water flushing, until the water washed out is for neutral, dried for standby under room temperature.Film is now even, and hardness and pliability are all relatively good.
10, the composite membrane made being put into concentration is in 80mg/L, 25ml lavo-ofloxacin solution, uses magnetic stirrer 30min under room temperature, is taken out by film, the fluorescence intensity of test solution.
For the treatment of simulation antibiotic Levofloxacin Wastewater, the fluorescence intensity before and after drug solution degraded adopts the test of F4500 type XRF, and maximum fluorescence excitation wavelength and emission wavelength are respectively 370nm, 500nm.After carrying out fluorescence intensity test, according to
calculate degradation rate, wherein, I
0for the fluorescence intensity of medicine waste water before treatment, I is the fluorescence intensity of the medicine waste water after film process, and the degradation rate calculated is 65.23%.
Detailed description of the invention 2
1, accurately measure glacial acetic acid 20ml in 1000ml volumetric flask, adding distil water constant volume, dose volume mark be 2% acetum for subsequent use.
2, get 0.5g Chitosan powder and be placed in 100ml beaker, add the acetum of 20ml2%, dissolve completely to shitosan by magnetic agitation, the transparent shape of solution, wiring solution-forming A.
3, get 0.10g lanthanum nitrate and be placed in 100ml beaker, add 20ml distilled water, lanthanum nitrate is dissolved completely, wiring solution-forming B.
4, solution A and B are blended in the beaker of another 100ml, add 1.6g glycerine, magnetic agitation 20h.Now the mass ratio of shitosan and lanthanum nitrate is 10:1, and qualities of glycerin concentration is 4%, and liquor capacity is 40ml, and the volume adding glycerine is ignored, and is designated as solution C.
5, C is placed in ultrasonic cleaning machine, sonic oscillation 20min, removes bubble.
6, accurately measure solution C, 4.0ml is in the glass culture dish of 6mm in diameter, sprawls evenly.
7, the culture dish completing film is placed in electric drying oven with forced convection, keeps 70 DEG C of dryings 10 hours, final obtained dry composite film.
8, prepare the NaOH solution that 1000ml mass concentration is 2%, add 20ml in culture dish, soak, until film separates with culture dish.
9, again by film distilled water flushing, until the water washed out is for neutral, dried for standby under room temperature.Film is now even, and hardness and pliability are all relatively good.
10, the composite membrane made being put into concentration is in 80mg/L, 30ml lavo-ofloxacin solution, uses magnetic stirrer 25min under room temperature, is taken out by film, the fluorescence intensity of test solution.Medicine degradation rate is 70.34%.
Detailed description of the invention 3
1, accurately measure glacial acetic acid 20ml in 1000ml volumetric flask, adding distil water constant volume, dose volume mark be 2% acetum for subsequent use.
2, get 0.5g Chitosan powder and be placed in 100ml beaker, add the acetum of 20ml2%, dissolve completely to shitosan by magnetic agitation, the transparent shape of solution, wiring solution-forming A.
3, get 0.15g lanthanum nitrate and be placed in 100ml beaker, add 20ml distilled water, lanthanum nitrate is dissolved completely, wiring solution-forming B.
4, solution A and B are blended in the beaker of another 100ml, add 2.0g glycerine, magnetic agitation 18h.Now the mass ratio of shitosan and lanthanum nitrate is 10:3, and qualities of glycerin concentration is 5%, and liquor capacity is 40ml, and the volume adding glycerine is ignored, and is designated as solution C.
5, C is placed in ultrasonic cleaning machine, sonic oscillation 40min, removes bubble.
6, accurately measure solution C, 4.5ml is in the glass culture dish of 6mm in diameter, sprawls evenly.
7, the culture dish completing film is placed in electric drying oven with forced convection, keeps 80 DEG C of dryings 8 hours, final obtained dry composite film.
8, prepare the NaOH solution that 1000ml mass concentration is 2%, add 20ml in culture dish, soak, until film separates with culture dish.
9, again by film distilled water flushing, until the water washed out is for neutral, dried for standby under room temperature.Film is now even, and hardness and pliability are all relatively good.
10, the composite membrane made being put into concentration is in 80mg/L, 20ml lavo-ofloxacin solution, uses magnetic stirrer 15min under room temperature, is taken out by film, the fluorescence intensity of test solution.Medicine degradation rate is 72.86%.
Detailed description of the invention 4
1, accurately measure glacial acetic acid 20ml in 1000ml volumetric flask, adding distil water constant volume, dose volume mark be 2% acetum for subsequent use.
2, get 0.5g Chitosan powder and be placed in 100ml beaker, add the acetum of 20ml2%, dissolve completely to shitosan by magnetic agitation, the transparent shape of solution, wiring solution-forming A.
3, get 0.20g lanthanum nitrate and be placed in 100ml beaker, add 20ml distilled water, lanthanum nitrate is dissolved completely, wiring solution-forming B.
4, solution A and B are blended in the beaker of another 100ml, add 3.2g glycerine, magnetic agitation 22h.Now the mass ratio of shitosan and lanthanum nitrate is 10:3, and qualities of glycerin concentration is 8%, and liquor capacity is 40ml, and the volume adding glycerine is ignored, and is designated as solution C.
5, C is placed in ultrasonic cleaning machine, sonic oscillation 50min, removes bubble.
6, accurately measure solution C, 5.0ml is in the glass culture dish of 6mm in diameter, sprawls evenly.
7, the culture dish completing film is placed in electric drying oven with forced convection, keeps 90 DEG C of dryings 6 hours, final obtained dry composite film.
8, prepare the NaOH solution that 1000ml mass concentration is 2%, add 20ml in culture dish, soak, until film separates with culture dish.
9, again by film distilled water flushing, until the water washed out is for neutral, dried for standby under room temperature.Film is now even, and hardness and pliability are all relatively good.
10, the composite membrane made being put into concentration is in 80mg/L, 15ml lavo-ofloxacin solution, uses magnetic stirrer 20min under room temperature, is taken out by film, the fluorescence intensity of test solution.Medicine degradation rate is 68.54%.
Each detailed description of the invention is test in laboratory above, and above preparation method and using method also can be generalized in production practices by those skilled in the art.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from principle of the present invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a preparation method for antibiotic adsorbed film, is characterized in that, described preparation method comprises the following steps:
Soluble chitosan is dissolved in the glacial acetic acid aqueous solution by step one, is designated as solution A;
Step 2 is water-soluble by lanthanum nitrate, wiring solution-forming, is designated as solution B;
Step 3 gets a certain amount of solution A and solution B mixing, adds glycerine and stirs, being designated as solution C;
Solution C is placed in culture dish by step 4, sprawls evenly, culture dish is put into drying box dry, makes dry composite film;
Dry composite film is separated with culture dish by step 5, makes antibiotic adsorbed film.
2. the preparation method of antibiotic adsorbed film as claimed in claim 1, it is characterized in that, described step one is specially and is dissolved in the glacial acetic acid aqueous solution of configure 2% by soluble chitosan, and magnetic agitation is dissolved completely to Chitosan powder, is designated as solution A.
3. the preparation method of antibiotic adsorbed film as claimed in claim 1, it is characterized in that, described step 3 is specially gets a certain amount of solution A and solution B mixing, wherein solution A quality mA is 10:1≤mA:mB≤10:3 with the ratio of the quality mB of solution B, add glycerine, magnetic agitation 24 hours, is designated as solution C, solution C is placed in ultrasonic cleaning machine, vibration 30min.
4. the preparation method of antibiotic adsorbed film as claimed in claim 1, it is characterized in that, described step 4 is specially and solution C is placed in culture dish, wherein the volume V of solution C is 3.5mL≤V≤5mL, culture dish uses 6cm glass culture dish, sprawls evenly, culture dish is put into electric drying oven with forced convection, 60 DEG C of dryings 12 hours, make dry composite film.
5. the preparation method of antibiotic adsorbed film as claimed in claim 1, it is characterized in that, described step 5 is specially and is separated with culture dish by dry composite film, and separation method is the NaOH solution immersion with 2%, dry composite film is separated with culture dish, makes antibiotic adsorbed film.
6. a using method for antibiotic adsorbed film, is characterized in that, described using method to drop in antibiotic waste water for antibiotic adsorbed film method described in any one of claim 1 to 5 made and stirs.
7. the using method of antibiotic adsorbed film as claimed in claim 6, is characterized in that, in described using method with antibiotic adsorbed film first with distilled water flushing to neutral, dry under room temperature, then to drop in antibiotic waste water and magnetic agitation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510855579.4A CN105268410B (en) | 2015-11-26 | 2015-11-26 | A kind of preparation method and application method of antibiotic adsorbed film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510855579.4A CN105268410B (en) | 2015-11-26 | 2015-11-26 | A kind of preparation method and application method of antibiotic adsorbed film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105268410A true CN105268410A (en) | 2016-01-27 |
| CN105268410B CN105268410B (en) | 2017-12-08 |
Family
ID=55138764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510855579.4A Active CN105268410B (en) | 2015-11-26 | 2015-11-26 | A kind of preparation method and application method of antibiotic adsorbed film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105268410B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108114703A (en) * | 2017-12-19 | 2018-06-05 | 湖北工程学院 | A kind of chitosan-rare earth composite membrane and preparation method and application |
| CN113637481A (en) * | 2021-07-23 | 2021-11-12 | 浙江大学 | Application of chitosan and derivatives thereof in reducing antibiotic resistance gene pollution in soil |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080176960A1 (en) * | 2002-06-19 | 2008-07-24 | National Institude Of Agrobiological Sciences | Biodegradable biopolymers, method for their preparation and functional materials constituted by these biopolymers |
| CN102492182A (en) * | 2011-12-07 | 2012-06-13 | 聊城大学 | Biofilms of rare-earth element contained chitosan and/or derivatives of chitosan |
| CN103801267A (en) * | 2014-02-11 | 2014-05-21 | 江苏大学 | Preparation method for novel magnetic chitosan composite microsphere antibiotic adsorbent |
| CN104045734A (en) * | 2014-07-08 | 2014-09-17 | 中国海洋大学 | Preparation method of resin having high-efficiency adsorption effect on patulin |
| CN104774290A (en) * | 2015-03-27 | 2015-07-15 | 南京师范大学 | PH and temperature dual-sensitive chitosan flocculating agent, and preparation method and application thereof |
-
2015
- 2015-11-26 CN CN201510855579.4A patent/CN105268410B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080176960A1 (en) * | 2002-06-19 | 2008-07-24 | National Institude Of Agrobiological Sciences | Biodegradable biopolymers, method for their preparation and functional materials constituted by these biopolymers |
| CN102492182A (en) * | 2011-12-07 | 2012-06-13 | 聊城大学 | Biofilms of rare-earth element contained chitosan and/or derivatives of chitosan |
| CN103801267A (en) * | 2014-02-11 | 2014-05-21 | 江苏大学 | Preparation method for novel magnetic chitosan composite microsphere antibiotic adsorbent |
| CN104045734A (en) * | 2014-07-08 | 2014-09-17 | 中国海洋大学 | Preparation method of resin having high-efficiency adsorption effect on patulin |
| CN104774290A (en) * | 2015-03-27 | 2015-07-15 | 南京师范大学 | PH and temperature dual-sensitive chitosan flocculating agent, and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 谢宇: "《壳聚糖及其衍生物制备与应用》", 31 July 2010 * |
| 赵文杰等: ""一种新型改性交联壳聚糖的制备及其对废水中四环素的去除机理"", 《山东大学学报（工学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108114703A (en) * | 2017-12-19 | 2018-06-05 | 湖北工程学院 | A kind of chitosan-rare earth composite membrane and preparation method and application |
| CN113637481A (en) * | 2021-07-23 | 2021-11-12 | 浙江大学 | Application of chitosan and derivatives thereof in reducing antibiotic resistance gene pollution in soil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105268410B (en) | 2017-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107082894B (en) | A kind of double-network hydrogel adsorbent and preparation method thereof and application as heavy metal absorbent | |
| CN102161781B (en) | Modified chitosan material capable of absorbing heavy metal ions and preparation method thereof | |
| CN106243282B (en) | Modification of chitosan/nano-cellulose composite aerogel and its preparation method and application | |
| CN106267300A (en) | A kind of multifunctional material having bactericidal haemostatic and biochemical war agent protective concurrently and preparation method thereof | |
| CN104257510B (en) | Preparation method based on layer assembly function nano microcapsule facial film | |
| CN107056986B (en) | Clean production process of chitosan-based super absorbent resin | |
| CN107540882A (en) | A kind of preparation method and application of multi function shell glycan composite sponge | |
| CN105268410A (en) | Preparation method and use method of antibiotic adsorption film | |
| CN107326650A (en) | A kind of method of modifying of terylene supatex fabric | |
| CN104492391B (en) | A kind of preparation method of chitosan-modified albumin nanospheres heavy-metal adsorption material | |
| CN104371127A (en) | Juicy food packaging biodegradable chitosan film preparation method | |
| CN103100376A (en) | Fiber natural polymeric adsorbent and application thereof | |
| CN102401818A (en) | High performance liquid chromatography determination method of tetracycline antibiotic in soil | |
| CN103191701B (en) | Preparation method of gold absorbent based on waste eggshell membrane biomaterial | |
| CN108514864B (en) | Chitin/graphene oxide composite sponge and preparation method and application thereof | |
| CN105062445A (en) | Interpenetrating polymer network modified pre-crosslinked profile control agent and preparation method thereof | |
| CN108097313A (en) | A kind of carbonitride/chitosan aeroge composite photo-catalyst and its preparation method and application | |
| CN107262051B (en) | Carboxymethyl Konjac Glucomannan microsphere adsorbing agent and preparation method thereof for dephosphorization | |
| Zeng et al. | Adsorption of Congo red by cross-linked chitosan resins | |
| CN100355790C (en) | Method for preparing transparent zinc hyaluronic acid | |
| CN105885068A (en) | Crosslinked chitosan membrane and application thereof | |
| CN104530437A (en) | Preparation method of cyclodextrin grafted chitosan polymer with water pollutant separating property | |
| CN104311848A (en) | Preparation method of regenerated fibroin-nano titanium oxide composite membrane | |
| US20160114528A1 (en) | Production technology of pet urinal pad having deammoniation function and high saline water absorption ability | |
| CN103272570B (en) | Preparation method and application of hemicellulose/chitosan/nano TiO2 hybrid material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |