CN107792911A - A kind of method for going in water removal to remain tetracycline using absorption method - Google Patents
A kind of method for going in water removal to remain tetracycline using absorption method Download PDFInfo
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- CN107792911A CN107792911A CN201711070366.6A CN201711070366A CN107792911A CN 107792911 A CN107792911 A CN 107792911A CN 201711070366 A CN201711070366 A CN 201711070366A CN 107792911 A CN107792911 A CN 107792911A
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- Prior art keywords
- resin
- tetracycline
- water
- remain
- metal ion
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of method for going in water removal to remain tetracycline, and more particularly, to a kind of method for going in water removal to remain tetracycline using absorption method, this method comprises the following steps：S1, resin pre-processed, to remove impurity；S2, by obtained by step S1 resin modified obtain metal ion support type resin；S3, by the metal ion support type resin obtained by step S2 be added to residual tetracycline water in, under the conditions of normal temperature, pH=4~8, adsorb 17~25h；S4, after the solid-liquid system obtained by step S3 is centrifuged, the content that tetracycline is remained in liquid phase is detected with high performance liquid chromatography；The inventive method is easy, and cost is relatively low, effect stability, reusable edible, and the removal to remaining tetracycline in any aqueous solution is applicable.
Description
Technical field
The present invention relates to a kind of method for going in water removal to remain tetracycline, goes to remove water using absorption method more particularly, to one kind
The method of middle residual tetracycline.
Background technology
Tetracycline antibiotics are a kind of broad-spectrum antibiotics as caused by actinomyces, including aureomycin, terramycin, tetracycline
Deng being mainly used in person poultry disease's preventing and treating and treatment, and feed addictive to promote growth of animal.Tetracycline antibiotics have
Ten dihydro aphthacene based structures, mainly prevent the growth metabolism of bacterium by suppressing the synthesis of bacterioprotein.
Tetracycline is one of current antibiotic most widely used in the world, and similar to other antibiotic, tetracycline is dynamic
Only have small part to be metabolized in thing alimentary canal, it is most of to be drained in the form of the mixture of parent compound and metabolin in excrement
Just or in urine, hence into soil, surface water, underground water, or even drinking water.In addition, tetracycline manufacturing enterprise production row
Waste water, because remaining the tetracycline of high concentration, and the significant contributor of environment tetracycline residue.
In recent years, with increase of the microorganism to tetracycline resistance, the processing of tetracycline wastewater is remained by increasingly
More concerns.The methods of being adsorbed at present using photocatalysis or microbial degradation, activated carbon or clay mineral matter is handled in water
Remain tetracycline.But because luminous intensity is serious with liquid layer thickness increase decay, make photocatalytic method be not suitable for handling liquid layer thickness compared with
The tetracycline remained in deep water system, and tetracycline strong antibacterial, has a broad antifungal spectrum, there is suppression to processing microorganism and kill and make
With, it is often more important that biodegradation process for treating, it is possible to produce drug-fast bacteria or drug resistant gene.
There is presently no the method for overcoming drawbacks described above.
The content of the invention
Easy it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of method, cost is relatively low, and effect is steady
It is fixed, reusable edible, and one kind that the removal to remaining tetracycline in any aqueous solution is applicable is gone in water removal using absorption method
The method for remaining tetracycline.
The present invention realizes by the following method：
A kind of method for going in water removal to remain tetracycline using absorption method, it is characterised in that：This method comprises the following steps：
S1, resin pre-processed, to remove impurity；
S2, by obtained by step S1 resin modified obtain metal ion support type resin；
S3, by the metal ion support type resin obtained by step S2 be added to residual tetracycline water in, in normal temperature, pH=
Under the conditions of 4~8,17~25h is adsorbed；
S4, after the solid-liquid system obtained by step S3 is centrifuged, is detected in liquid phase and remained with high performance liquid chromatography
The content of tetracycline；
Described resin preprocess method is：Elute resin to going out clarification of water with deionized water first, secondly with 0.8~
1.2mol/L hydrochloric acid solution elution 30~40min of resin, it is 6.8~7 to elute resin to water outlet pH value with deionized water, then
30~40min of resin is eluted with 0.8~1.2mol/L sodium hydroxide solution, is with deionized water elution resin to water outlet pH value
6.8~7, finally eluted with absolute ethyl alcohol and soak 3~6h, filter off liquid, 50~60 DEG C are dried in vacuum overnight, and produce；
The modified ion exchange resin that is used in the step S2 is commercially available macropore strong acid polystyrene cation
Exchanger resin D001-CC, metal ion Cu2+、Zn2+In any one；Metal ion load capacity：Cu2+Load capacity be 2~
6%th, Zn2+Load capacity is 16~21%；
Metal ion support type resin presses 10~40 times of throwings that tetracycline quality is remained in accessing pending water in the step S3
It is added in water；
The preparation method of the metal ion support type resin is：Pretreated resin is added to containing 0.2~
In 0.8mol/L hydrochloric acid solution and 0.02~0.1mol/L metal ion solutions, after 3~8h of stirring at normal temperature, 36~48h of standing,
With water filtering and washing 3~5 times, 12~24h is dried at 40~60 DEG C, you can.
The present invention has the following effects that：
1) method is easy：Method following steps provided by the invention：S1, resin pre-processed, to remove impurity；S2, general
Resin modified obtained by step S1 obtains metal ion support type resin；S3, by the metal ion support type tree obtained by step S2
Fat is added in the water of residual tetracycline, under the conditions of normal temperature, pH=4~8, adsorbs 17~25h；S4, by obtained by step S3
After solid-liquid system is centrifuged, the content that tetracycline is remained in liquid phase is detected with high performance liquid chromatography.
2) cost is relatively low, effect stability：Resin preprocess method is in the present invention：First resin is eluted with deionized water extremely
Go out clarification of water, secondly elute 30~40min of resin with 0.8~1.2mol/L hydrochloric acid solution, resin is eluted extremely with deionized water
Water outlet pH value is 6.8~7, then elutes 30~40min of resin with 0.8~1.2mol/L sodium hydroxide solution, uses deionization
Water wash resin to water outlet pH value is 6.8~7, is finally eluted with absolute ethyl alcohol and soaks 3~6h, elimination liquid, 50~60 DEG C
It is dried in vacuum overnight, produces；The modified ion exchange resin that is used in the step S2 is commercially available macropore strong acid benzene second
Alkene cation exchanger resin D001-CC, metal ion Cu2+、Zn2+In any one；Metal ion load capacity：Cu2+It is negative
Carrying capacity is 2~6%, Zn2+Load capacity is 16~21%；Metal ion support type resin in water by remaining Fourth Ring in the step S3
10~40 times of quality amount are added in water；The preparation method of the metal ion support type resin is：By pretreated tree
Fat is added in the hydrochloric acid solution containing 0.2~0.8mol/L and 0.02~0.1mol/L metal ion solutions, and stirring at normal temperature 3~
8h, after standing 36~48h, with water filtering and washing 3~5 times, 12~24h is dried at 40~60 DEG C, you can.Absorption method is a kind of
Effectively, the method for the economic numerous pollutants of removal.The small, technique of this method investment is simple and convenient to operate, manageability, can be compared with
Good carries out process modification to original sewage plant.And in numerous adsorbent ion exchange resins due to its good regeneration
Performance and receive much attention.Ion exchange resin is modified, metal ion is attached on resin by ion exchange, so as to
Metal ion is set to turn into the active site of later separation.Metal ion can coordinate with elements such as N, O on tetracycline molecule
Reaction, and then improve the adsorptive selectivity to tetracycline.
3) tetracycline clearance is high, applied widely：Method provided by the invention can be known as very to remaining Fourth Ring in water
Good clearance, its method is easy, and cost is relatively low, effect stability, reusable edible, and is removed to remaining tetracycline in any water
It is applicable.After testing, the aqueous of residual tetracycline is handled by the inventive method, tetracycline clearance reaches 97~99%.
4) cost of raw material is cheap, reusable edible：Using cheap commercially available macropore strong acid polystyrene sun from
The Cu of sub-exchange resin and wide material sources2+、Zn2+For raw material, metal ion support type resin sorbent is prepared.The adsorbent is inhaled
After attached tetracycline, then through the adsorbed tetracycline of butyl acetate or ethyl acetate extraction desorption, the resin adsorption after desorption processing
Agent reusable edible.
5) there is good economy and environmental benefit：Resin sorbent after tetracycline adsorption, Fourth Ring can be obtained through desorption
Plain product, thus there is certain economic benefit, while unfavorable shadow of the discharge to environment because remaining tetracycline water sample can be reduced or remitted
Ring, there is good environmental benefit.
Embodiment
In order that objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further
Describe in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair
It is bright.
Resin preprocess method is in the embodiment of the present invention：
Resin is eluted to going out clarification of water with deionized water first；Secondly tree is eluted with 0.8~1.2mol/L hydrochloric acid solution
30~40min of fat, it is 6.8~7 to elute resin to water outlet pH value with deionized water；Then with 0.8~1.2mol/L hydroxide
Sodium solution elutes 30~40min of resin, and it is 6.8~7 to elute resin to water outlet pH value with deionized water；Finally drenched with absolute ethyl alcohol
Wash and soak 3~6h, filter off liquid, 50~60 DEG C are dried in vacuum overnight, and produce.
Resin and metal ion type used is in the embodiment of the present invention：
It is commercially available large hole strong acid styrene system cation exchange resin D001- for modified ion exchange resin
CC, metal ion Cu2+、Zn2+Middle a certain kind, metal ion load capacity：Cu2+Load capacity is 2~6%, Zn2+Load capacity is 16
~21%.
Metal ion support type process for preparing resins is in the embodiment of the present invention：
Pretreated resin is added to hydrochloric acid solution and 0.02~0.1mol/L metal ions containing 0.2~0.8mol/L
In solution, 3~8h of stirring at normal temperature, after standing 36~48h, with water filtering and washing 3~5 times, dry 12 at 40~60 DEG C~
24h, produce.
Embodiment 1：A kind of method for going in water removal to remain tetracycline using absorption method, this method are to take residual tetracycline
Aqueous, pH 5, Fourth Ring cellulose content are 400mg/L, and its processing procedure is：The aqueous 1000ml of residual 400mg/L tetracyclines is taken,
Add 4g loads 3.8%Cu2+Modified resin, 25h being adsorbed at normal temperatures, being centrifuged, liquid is detected with high performance liquid chromatography
Fourth Ring cellulose content is remained in phase, the clearance of tetracycline is 97% in water.
Embodiment 2：A kind of method for going in water removal to remain tetracycline using absorption method, this method are to take residual tetracycline
Aqueous, pH 7, Fourth Ring cellulose content are 300mg/L.Its processing procedure is：The aqueous 1000ml of residual 300mg/L tetracyclines is taken,
Add 6g loads 18.0%Zn2+Modified resin.19h is adsorbed at normal temperatures, is centrifuged, and liquid is detected with high performance liquid chromatography
Fourth Ring cellulose content is remained in phase, the clearance of tetracycline is 98% in water.
Embodiment 3：A kind of method for going in water removal to remain tetracycline using absorption method, this method are to take residual tetracycline
Aqueous, pH 6, Fourth Ring cellulose content are 100mg/L.Its processing procedure is：The aqueous 1000ml of residual 100mg/L tetracyclines is taken,
Add 4g loads 3.2%Cu2+Modified resin.21h is adsorbed at normal temperatures, is centrifuged, and liquid is detected with high performance liquid chromatography
Fourth Ring cellulose content is remained in phase, the clearance of tetracycline is 99% in water.
Described above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (5)
- A kind of 1. method for going in water removal to remain tetracycline using absorption method, it is characterised in that：This method comprises the following steps：S1, resin pre-processed, to remove impurity；S2, by obtained by step S1 resin modified obtain metal ion support type resin；S3, by the metal ion support type resin obtained by step S2 be added to residual tetracycline water in, in normal temperature, pH=4~8 Under the conditions of, adsorb 17~25h；S4, after the solid-liquid system obtained by step S3 is centrifuged, is detected with high performance liquid chromatography in liquid phase and remain Fourth Ring The content of element.
- A kind of 2. method for going in water removal to remain tetracycline using absorption method as claimed in claim 1, it is characterised in that：It is described Resin preprocess method is：Resin is eluted to clarification of water is gone out with deionized water first, and next is molten with 0.8~1.2mol/L hydrochloric acid Liquid elutes 30~40min of resin, and it is 6.8~7 to elute resin to water outlet pH value with deionized water, then with 0.8~1.2mol/L Sodium hydroxide solution elution 30~40min of resin, with deionized water elute resin to water outlet pH value be 6.8~7, finally with nothing Water-ethanol elutes and soaks 3~6h, filters off liquid, 50~60 DEG C are dried in vacuum overnight, and produce.
- A kind of 3. method for going in water removal to remain tetracycline using absorption method as claimed in claim 1, it is characterised in that：It is described The modified ion exchange resin that is used in step S2 is large hole strong acid styrene system cation exchange resin D001-CC, gold Category ion is Cu2+、Zn2+In any one；Metal ion load capacity：Cu2+Load capacity is 2~6%, Zn2+Load capacity be 16~ 21%.
- A kind of 4. method for going in water removal to remain tetracycline using absorption method as claimed in claim 1, it is characterised in that：It is described Metal ion support type resin is added in water by 10~40 times that tetracycline quality is remained in accessing pending water in step S3.
- A kind of 5. method for going in water removal to remain tetracycline using absorption method as claimed in claim 1, it is characterised in that：It is described The preparation method of metal ion support type resin is：It is molten that pretreated resin is added to the hydrochloric acid containing 0.2~0.8mol/L In liquid and 0.02~0.1mol/L metal ion solutions, after 3~8h of stirring at normal temperature, 36~48h of standing, with water filtering and washing 3~5 It is secondary, 12~24h is dried at 40~60 DEG C, you can.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993390A (en) * | 2018-08-10 | 2018-12-14 | 宁夏大学 | A method of utilizing residual tetracycline in pharmacy waste water after ZnO support type expanded graphite removal flocculation treatment |
| CN108993389A (en) * | 2018-08-10 | 2018-12-14 | 宁夏大学 | It is a kind of to utilize MnO2The method of tetracycline is remained after the removal flocculation of support type graphene in pharmacy waste water |
| CN111995789A (en) * | 2020-03-25 | 2020-11-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN112960793A (en) * | 2019-12-12 | 2021-06-15 | 芜湖沃泰环保科技有限公司 | System for removing antibiotics from water body |
| CN114085829A (en) * | 2021-11-18 | 2022-02-25 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Efficient enrichment method for viruses in environmental medium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993390A (en) * | 2018-08-10 | 2018-12-14 | 宁夏大学 | A method of utilizing residual tetracycline in pharmacy waste water after ZnO support type expanded graphite removal flocculation treatment |
| CN108993389A (en) * | 2018-08-10 | 2018-12-14 | 宁夏大学 | It is a kind of to utilize MnO2The method of tetracycline is remained after the removal flocculation of support type graphene in pharmacy waste water |
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| CN112960793A (en) * | 2019-12-12 | 2021-06-15 | 芜湖沃泰环保科技有限公司 | System for removing antibiotics from water body |
| CN111995789A (en) * | 2020-03-25 | 2020-11-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN111995789B (en) * | 2020-03-25 | 2022-09-27 | 武汉纺织大学 | Hydrophilic resin for catalytic degradation of antibiotics and preparation method and application thereof |
| CN114085829A (en) * | 2021-11-18 | 2022-02-25 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Efficient enrichment method for viruses in environmental medium |
| CN114085829B (en) * | 2021-11-18 | 2023-08-11 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Efficient enrichment method for viruses in environmental medium |
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