CN115337898B - Preparation method and application of diatomite-supported basic zinc chloride - Google Patents
Preparation method and application of diatomite-supported basic zinc chloride Download PDFInfo
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- CN115337898B CN115337898B CN202210515215.1A CN202210515215A CN115337898B CN 115337898 B CN115337898 B CN 115337898B CN 202210515215 A CN202210515215 A CN 202210515215A CN 115337898 B CN115337898 B CN 115337898B
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 title claims abstract description 90
- 235000005074 zinc chloride Nutrition 0.000 title claims abstract description 45
- 239000011592 zinc chloride Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 238000005119 centrifugation Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 3
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 claims description 38
- 229960003405 ciprofloxacin Drugs 0.000 claims description 19
- 238000001179 sorption measurement Methods 0.000 abstract description 27
- 239000003242 anti bacterial agent Substances 0.000 abstract description 11
- 229940088710 antibiotic agent Drugs 0.000 abstract description 11
- 239000003463 adsorbent Substances 0.000 abstract description 8
- 230000008929 regeneration Effects 0.000 abstract description 4
- 238000011069 regeneration method Methods 0.000 abstract description 4
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 239000000463 material Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000011521 glass Substances 0.000 description 7
- 238000011068 loading method Methods 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000005909 Kieselgur Substances 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229960001229 ciprofloxacin hydrochloride Drugs 0.000 description 4
- DIOIOSKKIYDRIQ-UHFFFAOYSA-N ciprofloxacin hydrochloride Chemical compound Cl.C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 DIOIOSKKIYDRIQ-UHFFFAOYSA-N 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000013068 control sample Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000588747 Klebsiella pneumoniae Species 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940124350 antibacterial drug Drugs 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229940124307 fluoroquinolone Drugs 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 239000012629 purifying agent Substances 0.000 description 1
- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical compound C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/024—Compounds of Zn, Cd, Hg
- B01J20/0244—Compounds of Zn
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to the technical field of water body treatment, in particular to a preparation method and application of diatomite-supported basic zinc chloride, which comprises the following steps: s1, diatomite pretreatment; s2, mixing the diatomite treated in the step S1 with zinc chloride according to the proportion, and dissolving the mixture in a dilute hydrochloric acid solution to form a mixed solution; then dropwise adding sodium hydroxide solution into the solution, continuously stirring for 15-20 min, and standing to obtain suspension; s3, centrifuging the suspension obtained in the step S2, and drying, grinding and sieving the solid obtained by centrifugation to obtain the composite material. The synthesis method is simple, the reaction condition is mild, the adsorption performance is good, the adsorption is promoted due to the fact that the synthesis method has a large number of hydroxyl functional groups, and the pollutant adsorption efficiency is high; the adsorbent has good regeneration performance, can be repeatedly used, and effectively reduces cost. The diatomite loaded basic zinc chloride adsorbent can be applied to the field of adsorbing water antibiotics and has huge potential application value.
Description
Technical Field
The invention relates to the technical field of water body treatment, in particular to a preparation method and application of diatomite-supported basic zinc chloride.
Technical Field
Antibiotics are an emerging pollutant, and pollution to water environment has become an environmental problem of global concern. Antibiotics are widely used in the fields of human medicine, animal husbandry and agriculture for the control of bacterial infections. However, due to their high usage and environmental durability, antibiotics induce the production of drug resistant strains and antibiotic resistance genes. Among them, ciprofloxacin (CIP) is the highest of fluoroquinolones currently used clinically as a third-generation quinolone broad-spectrum antibacterial drug, and has antibacterial activity against gram-negative bacilli in vitro. However, it has been shown that ciprofloxacin is one of the antibiotics with the highest drug resistance rate for bacteria such as Escherichia coli, pseudomonas aeruginosa, klebsiella pneumoniae subspecies, and the like. The generation of drug-resistant bacteria and the transmission of drug-resistant genes seriously threaten public health. Thus, the removal of antibiotics has become one of the important challenges in the environmental field.
At present, the methods for removing antibiotics mainly comprise a chemical method, a biological method, a membrane separation technology and an adsorption method. The chemical method changes the chemical structure of the antibiotics through chemical reaction, degrades and mineralizes even pollutants to achieve the aim of removing, but is easily influenced by the type, pH, temperature and the like of the oxidant, and the oxidant has high cost and is easy to cause secondary pollution. Biological methods have better removal of most antibiotics in water, however, their degradation rates are slower and drug-resistant bacteria and superbacteria are easily produced. The membrane separation technology is a novel treatment technology, and the research on the degradation path and mechanism of antibiotics is not mature. The adsorption method has the characteristics of simple operation, higher removal rate and repeated utilization, and has wide application prospect and profound research significance.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method and application of diatomite-supported basic zinc chloride.
The aim of the invention is realized by the following technical scheme:
the preparation method of the diatomite-supported basic zinc chloride comprises the following steps:
s1, diatomite pretreatment;
s2, mixing the diatomite treated in the step S1 and zinc chloride according to the proportion of 5-9:10, and dissolving the mixture in a dilute hydrochloric acid solution to form a mixed solution with the total mass fraction of 1-4%; then dropwise adding 0.4mol/L sodium hydroxide solution into the solution, continuously stirring for 15-20 min, and standing for 10-20 min to obtain suspension;
s3, centrifuging the suspension obtained in the step S2, and drying, grinding and sieving the solid obtained by centrifugation to obtain the composite material.
Diatomaceous earth is an effective adsorbent. Diatomite is siliceous rock mainly composed of diatomite remains, has a layered structure composed of silicon oxygen tetrahedra and aluminum oxygen octahedra, contains a large number of micropores and has large specific surface area, so that the diatomite has huge adsorption potential. However, the diatomite has more impurities in raw ore, and the adsorption performance of the diatomite is limited. The diatomite is subjected to inorganic modification treatment, and mainly inorganic macromolecule modifier is added to uniformly disperse the diatomite between diatomite pore channels to form a column-layer association structure, dredge or expand the diatomite pore channels, and form larger spaces among association particles so as to accommodate more adsorbants, so that the aim of improving the adsorption capacity of the diatomite is finally achieved.
Basic zinc chloride fractionThe sub formula is Zn 5 Cl 2 (OH) 8 ·H 2 O is white particles or powder, is not hygroscopic and is difficult to dissolve in water, and has a certain adsorption effect. Therefore, the adsorption performance of the diatomite can be improved by loading the diatomite with basic zinc chloride.
Preferably, the concentration of the sodium hydroxide solution in the step S2 is 0.1-0.4 mol/L; the usage amount of the sodium hydroxide solution is 42-48% of the volume of the mixed solution.
Preferably, in the step S3, the centrifugal process uses a rotational speed of 3800-5000 r/min, and the centrifugal time is 8-15 min.
Preferably, in the step S3, the drying process is performed at a temperature of 50 to 65 ℃ for 20 to 30 hours.
Preferably, in the step S3, the sieving is performed with a mesh size of 150 to 300 mesh.
The diatomite loaded basic zinc chloride is prepared by the preparation method of the diatomite loaded basic zinc chloride.
The diatomite loaded basic zinc chloride is applied to water purifying agents.
Preferably, the diatomite loaded basic zinc chloride is used for removing antibiotics in water.
Preferably, the antibiotic is ciprofloxacin.
Preferably, when the diatomite loaded basic zinc chloride is used for removing water, the pH of the water body of the ciprofloxacin is 3-11.
Compared with the prior art, the invention has the following technical effects:
1. the diatomite loaded basic zinc chloride material plays roles of adsorption of diatomite and adsorption and modification of basic zinc chloride, so that the material has good adsorption performance, good stability and dispersibility and high removal efficiency of ciprofloxacin in water. Experiments prove that when the environment condition is 25 ℃, the load ratio of basic zinc chloride is 45%, and the equilibrium adsorption quantity reaches 831.96mg/g.
2. In the existing adsorbent capable of adsorbing and removing ciprofloxacin in water, the invention has higher removal efficiency and higher speed; compared with other adsorption methods, the method has the advantages of low production cost, simple operation, no secondary pollution and the like, can be used for the second time, and has the potential of being put into application.
Drawings
FIG. 1 is an XRD pattern of diatomaceous earth loaded with basic zinc chloride and diatomaceous earth of a control sample;
FIG. 2 is a FTIR plot of diatomaceous earth loaded with basic zinc chloride versus control sample diatomaceous earth;
fig. 3 is a graph showing the effect of diatomite-supported basic zinc chloride on ciprofloxacin removal.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail with reference to specific examples and comparative examples. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
Except for the special description, the equipment used in the embodiment is conventional experimental equipment, and the materials and reagents used are all obtained in the market unless the special description is made, and the experimental method without the special description is also conventional experimental method.
Example 1
The preparation method of the diatomite loaded basic zinc chloride material comprises the following steps:
1. 3.09g of zinc chloride and 2.75g of diatomite are weighed for later use;
2. 100ml of water is added and stirred, and 113.625ml of 0.2mol/L NaOH solution is dropwise added, and stirring is continued during the period;
3. the suspension is equally arranged in four 100ml glass bottles, the rotating speed is set to 4000r/min, the time is set to 10min, and the glass bottles are put into a low-speed centrifuge for centrifugation for five times;
4. putting the mixture into a blast drying box, setting the temperature to be 60 ℃ and setting the time to be 24 hours;
5. and after the drying is finished, taking out the solid powder from the agate mortar, grinding the solid powder into fine powder, and sieving the fine powder with a 200-mesh sieve to obtain a loaded sample.
The loading is 45% (calculated by zinc hydroxide), and the dosage of the zinc chloride and the diatomite is adjusted according to different loading.
Experimental example 1
XRD and FTIR characterization were performed on diatomite-supported basic zinc chloride and control sample diatomite, respectively, and the results are shown in FIG. 1 and FIG. 2, respectively.
In fig. 1, the diatomite-supported basic zinc chloride material has sharp peaks near 2θ=21.9°, which are main characteristic peaks of diatomite; comparing the standard sample picture (PDF#07-0155) of basic zinc chloride, the prepared diatomite loaded basic zinc chloride material contains main characteristic peaks of basic zinc chloride; in addition, the XRD pattern of the diatomite loaded basic zinc chloride material is similar to that of natural diatomite, which shows that the crystal structure of the diatomite is not destroyed by the loading.
In FIG. 2, absorption peaks appear near 700-760 cm-1 and 1076cm-1 of the diatomite loaded basic zinc chloride material, which are formed by Si-O stretching vibration in amorphous SiO2, but the absorption peak of stretching vibration of-OH appears near 3500cm-1 is weakened compared with the strong peak of the diatomite sample, and the absorption peak is enhanced compared with the diatomite sample after the basic zinc chloride is introduced. The result shows that the diatomite loaded basic zinc chloride material has rich functional groups on the surface, hydrogen atoms in-OH can form hydrogen bonds among substance molecules, so that the adsorption effect is promoted, and the loaded basic zinc chloride and the diatomite are better combined.
Experimental example 2
The effect of the adsorbent load ratio on ciprofloxacin adsorption was tested as follows:
1. preparing diatomite loaded basic zinc chloride adsorbent with 15%,30%,45% and 60% of loading (calculated by zinc hydroxide) respectively;
2. sequentially weighing 10mg of adsorbents with different loading ratios, and adding into a 50ml glass bottle;
3. sequentially adding 20ml of 500mg/L ciprofloxacin solution;
4. placing into a shaking table, setting the temperature to 25 ℃, setting the rotating speed to 150r/min, and setting the time to 24 hours;
5. taking out the glass bottle from the shaking table, and centrifuging for 10min at 4000 r/min;
6. sucking the liquid in the centrifuged bottle by using a disposable needle, and filtering by using a 0.22 mu m filter membrane;
7. the residual concentration of ciprofloxacin was detected by an ultraviolet spectrophotometer, its absorbance was measured at 272nm, and the data was recorded and processed.
The experimental results are shown in table 1. From the experimental results, it was found that the adsorption amount reached 2172.23mg/g (in terms of adsorption amount divided by the load ratio) best when the load ratio was 45%.
TABLE 1
Experimental example 3
The effect of pH on ciprofloxacin adsorption was determined as follows:
1. taking 0.25g ciprofloxacin hydrochloride in a 500ml volumetric flask, and preparing 500mg/L ciprofloxacin solution; 2. transferring the ciprofloxacin solution to 9 100ml volumetric flasks to fix the volume;
3. respectively adjusting the PH to 3, 4, 5, 6, 7, 8, 9, 10 and 11; error range + -0.1;
4. putting 20ml of the solution into a 50ml glass bottle in each volumetric flask, and adding 10mg of diatomite loaded basic zinc chloride powder;
5. placing into a shaking table, setting the temperature to 25 ℃, setting the rotating speed to 150r/min, and setting the time to 24 hours;
6. taking out the glass bottle from the shaking table, and centrifuging for 10min at 4000 r/min;
8. sucking the liquid in the centrifuged bottle by using a disposable needle, and filtering by using a 0.22 mu m filter membrane;
9. the residual concentration of ciprofloxacin was detected by an ultraviolet spectrophotometer, its absorbance was measured at 272nm, and the data was recorded and processed.
The experimental results are shown in table 2. From the experimental results, the diatomite loaded basic zinc chloride achieves the maximum adsorption capacity at the pH=7, and the adsorption capacity is not greatly influenced by the pH at the pH=3-10, and the adsorption effect very similar to the optimal pH can be achieved by adopting the condition of not adjusting the pH, namely, the pH=5.14.
TABLE 2 adsorption of ciprofloxacin by diatomite-supported basic Zinc chloride materials at different pH values
Experimental example 4
The regeneration effect of the diatomite loaded basic zinc chloride adsorbent is tested, and the specific steps are as follows:
1. preparing ciprofloxacin hydrochloride solution with initial concentration of 100 mg/L;
2. 10mg of diatomite loaded basic zinc chloride and 20ml of ciprofloxacin hydrochloride solution are added into a 50ml glass bottle;
3. placing into a shaking table, setting the rotating speed to 200r/min, the temperature to 25 ℃ and the setting time to 24h;
4. when the process is finished, centrifuging at 4000r/min for 10 minutes, adding 20ml of ethanol, fully shaking and uniformly mixing, and centrifuging once;
5. removing supernatant, adding 20ml of absolute ethyl alcohol and placing into a shaking table for 24 hours;
6. repeating the centrifugation step, removing supernatant, and drying in a 60 ℃ oven until the weight is constant;
7. weighing the residual solid, and confirming the added ciprofloxacin hydrochloride solution according to the first solid-to-liquid ratio; the experiment was repeated five times to determine absorbance and adsorption efficiency.
The removal effect of the diatomite loaded basic zinc chloride on ciprofloxacin is shown in figure 3. The result shows that the adsorption efficiency reaches 75% when the second regeneration is carried out; the adsorption efficiency reaches 65% when the fifth regeneration is carried out.
Finally, it should be noted that the above-mentioned embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. The application of diatomite-supported basic zinc chloride in removing ciprofloxacin in water is characterized in that the preparation method of the diatomite-supported basic zinc chloride comprises the following steps:
s1, diatomite pretreatment;
s2, mixing the diatomite treated in the step S1 and zinc chloride according to the mass ratio of 5-9:10, and dissolving the mixture in a dilute hydrochloric acid solution to form a mixed solution with the total mass fraction of 1-4%; then dropwise adding sodium hydroxide solution into the solution, continuously stirring for 15-20 min, and standing for 10-20 min to obtain suspension;
s3, centrifuging the suspension obtained in the step S2, and drying, grinding and sieving the solid obtained by centrifugation to obtain the solid; the drying process is carried out for 20-30 hours at the temperature of 50-65 ℃.
2. The use according to claim 1, characterized in that the concentration of sodium hydroxide solution in step S2 is 0.4mol/L; the usage amount of the sodium hydroxide solution is 42-48% of the volume of the mixed solution.
3. The use according to claim 1, wherein in step S3, the centrifugation is performed at a rotational speed of 3800-5000 r/min for a period of 8-15 min.
4. The use according to claim 1, wherein in step S3, the sieving is performed with a mesh size of 150-300 mesh.
5. The use according to claim 1, wherein the pH of the water body of ciprofloxacin is 3 to 11.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091591A (en) * | 2010-12-29 | 2011-06-15 | 广东工业大学 | Kieselguhr modified adsorption material and preparation method and application thereof |
| CN103316628A (en) * | 2013-06-27 | 2013-09-25 | 昆明理工大学 | Preparation method and application of adsorbent |
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| CN110975798A (en) * | 2019-11-13 | 2020-04-10 | 浙江大学 | Preparation method, application and regeneration method of FeO (OH) -diatomite composite adsorbent |
| CN112169755A (en) * | 2020-09-24 | 2021-01-05 | 武汉理工大学 | Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water |
| CN113813921A (en) * | 2021-09-30 | 2021-12-21 | 华东交通大学 | Preparation method and application of lysine functionalized layered double hydroxide adsorbent |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091591A (en) * | 2010-12-29 | 2011-06-15 | 广东工业大学 | Kieselguhr modified adsorption material and preparation method and application thereof |
| CN103316628A (en) * | 2013-06-27 | 2013-09-25 | 昆明理工大学 | Preparation method and application of adsorbent |
| CN109527340A (en) * | 2019-01-02 | 2019-03-29 | 中国科学院兰州化学物理研究所 | A kind of silicates functional form mold toxin sorbent |
| CN110227416A (en) * | 2019-06-24 | 2019-09-13 | 武汉理工大学 | A kind of preparation and its application in fluoroquinolone antibiotics removal in water of iron zinc and phosphoric acid modification sludge organism charcoal |
| CN110975798A (en) * | 2019-11-13 | 2020-04-10 | 浙江大学 | Preparation method, application and regeneration method of FeO (OH) -diatomite composite adsorbent |
| CN112169755A (en) * | 2020-09-24 | 2021-01-05 | 武汉理工大学 | Preparation method of hydrothermally synthesized zinc chloride activated magnetic sludge biochar applied to tetracycline removal in water |
| CN113813921A (en) * | 2021-09-30 | 2021-12-21 | 华东交通大学 | Preparation method and application of lysine functionalized layered double hydroxide adsorbent |
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