CN102125819B - Iron-loaded cotton fiber material and preparation method thereof - Google Patents
Iron-loaded cotton fiber material and preparation method thereof Download PDFInfo
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- CN102125819B CN102125819B CN 201110051205 CN201110051205A CN102125819B CN 102125819 B CN102125819 B CN 102125819B CN 201110051205 CN201110051205 CN 201110051205 CN 201110051205 A CN201110051205 A CN 201110051205A CN 102125819 B CN102125819 B CN 102125819B
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Abstract
The invention discloses an iron-loaded cotton fiber material with absorbent cotton fiber as basic skeleton and a preparation method thereof, belonging to the technical field of macromolecular material. The fiber material structurally contains the hydroxide of amorphous iron. The preparation method thereof comprises the steps of: taking the absorbent cotton fiber as the basic skeleton, loading ferric iron salt solution through dispersion and hydrolysis so that the structure of the fiber contains the hydroxide of amorphous iron. The reaction process is simple, the conditions are moderate, and the reaction agents adopted are nontoxic and environmentally-friendly. The fiber material keeps fibrous shape of the absorbent cotton fiber, has stable performance in air, and causes no pH change of water when being used as adsorbent in the water, and the iron-loaded shape of the adsorbent is stable so that arsenite ions in the water can be adsorbed effectually.
Description
Technical field
The present invention relates to a kind of fibrous material, relate in particular to a kind of year iron cotton fibre material and preparation method thereof, belong to technical field of polymer materials.
Background technology
Because having stronger absorption to inorganic ions such as arsenic and fluorine, some metal oxide or hydroxide removes ability; Therefore; These metal oxides or hydroxide are loaded on some carriers, become this area research focus thereby prepare some inorganic anion sorbing materials metal oxide-loaded or hydroxide.At present, the carrier material that is used for carrying iron adsorbent can be divided into basically: (1) natural minerals and inorganic material.Like CN200610078899 " a kind of cubic sulfate lepidocrocite preparation of adsorbent method that is used for arsenic removal "; CN200610008135 " a kind of preparation of iron-managanese compounded oxide/diatomite adsorbant, use and renovation process " and Yan Yingtao etc. have reported preparation method's (Chang An University's journal, 2004 years 03 phases) of a kind of year iron silica gel; (2) active carbon and NACF.Like CN200510110226 " preparation method of iron carrying active carbon dearsenic adsorber ", and HRISTOVSKI etc. (Journal of Environmental Science and Health, Part A (2009) 44; 354 – 361) and Zhang etc. (Carbon; Volume 48, and Issue 1, and January 2010; Pages 60-67) to relate to the NACF be that preparing carriers is carried iron adsorbent such as KIM etc. (Journal of Environmental Science and Health to document; Part A (2010) 45,177 – 182), relating to the granular active carbon is the preparing carriers adsorbent.(3) natural macromolecular material." carry iron ball shape cellulose adsorbent and preparation and application " like CN1593745A, CN1589959A " the iron ligand exchange cotton fiber preparation of adsorbent method of carrying of high selectivity ", Guo etc. (Environ. Sci. Technol.; 2005,39 (17), pp 6808 – 6818); Having studied with the gossypin is that matrix material prepares adsorbent, and Altundogan etc. (Process Biochemistry., Volume 40; Issues 3-4, March 2005, Pages 1443-1452) iron is loaded on the betaine slurry; Iron adsorbent is carried in preparation, and Dupont etc. (Environmental Chemistry Letters, Volume 5; Number in August, 3/2007) be the preparing carriers adsorbent with the lignocellulosic, Katsutoshi etc. (Kagaku Kogaku Ronbunshu, VOL.29; NO.3; PAGE.389-394 (2003)) be the preparing carriers adsorbent with crosslinked pectic acid.(4) macromolecular material after the modification.Like CN200910028414 " composite cationic ion-exchange resin supporting iron-series duplex metal nano granules "; Rau etc. (Journal of Radioanalytical and Nuclear Chemistry, Volume 246, Number in December, 3/2000); Shao etc. (Hydrometallurgy, Volume 91, Issues 1-4; March 2008; Pages 138-143), Pan etc. (Water Research, 44 (2010) the 815 – 824) adsorbent that has been preparing carriers with the resin material; Lin etc. (Environmental Engineering Science; Volume 26; Number 11; 2009), Vatutsina etc. (Reactive & Functional Polymers 67 (2007) 184 – 201) is with functional polymer fibre material be preparing carriers adsorbent etc.
In above-mentioned carrier material, because cotton fiber is a kind of natural, recyclable materials, this carrier good hydrophilic property, porosity is big, has been widely used as bioactive materials.Carrying iron with cotton fiber as carrying iron material, in present research, how through crosslinked, is that carrier carries iron with spherical cellulose; Like CN1593745A, CN1589959A, Guo etc. (Environ. Sci. Technol.; 2005,39 (17), pp 6808 – 6818) etc. in report.And, do not change the fiber condition of cotton fibre material for being carrier with the cotton fiber, the research that iron loads on the cotton fibre material is fewer.At present, because flourish and the tangible unique advantage of fibrous material such as specific area is big, circulating resistance is little, can use in a variety of forms etc., a feasible year iron fiber shape sorbing material will have bigger application and development potentiality.
Summary of the invention
The object of the invention is to provide that a kind of fiber condition that does not change cotton fibre material has that hydrophily is strong concurrently, good mechanical property, advantages of good adsorption effect carry the iron fiber adsorbent; Another purpose of the present invention is to provide its preparation method.
For realizing the object of the invention, be carrier with the natural macromolecular material cotton fiber, through simple, gentle, eco-friendly synthetic route, prepare the high year iron fiber adsorbent of a kind of iron content to realize technical scheme of the present invention.
The present invention carry the iron fiber adsorbent with degreasing cotton fiber as basic skeleton, contain the iron hydroxide that exists with amorphous state, and kept the fibrous form of degreasing cotton fiber.
Its synthetic method is: with degreasing cotton fiber washing, be immersed in mass percent and be 2% ~ 10%, temperature is in 10 ~ 50 ℃ the ferric iron aqueous solution, after 1 ~ 3 hour; Stir; The aqueous slkali that dropwise adds 0.5 ~ 2M, trivalent iron salt through disperse, hydrolysis is written into absorbent cotton, in air, leave standstill 3 ~ 8 hours after; Water is washed till neutrality, in 30 ~ 80 ℃ of oven dry.Iron content increases along with the increase of carrying the iron number of times, and the fiber weightening finish is controlled at 10% ~ 40%.
The degreasing cotton fiber that the present invention adopted is a commercial goods level absorbent cotton, and filament length is at 3 ~ 7cm, and the tension brute force is 0.021 ~ 0.054N.Used ferric iron solution is iron chloride, ferric sulfate, iron nitrate solution etc.Used aqueous slkali is NaOH, ammoniacal liquor etc.The ferric iron aqueous solution is 1:3 with aqueous slkali maximum volume ratio.
Beneficial effect of the present invention is: (1) raw material degreasing cotton fiber wide material sources, performance quality is stable.(2) course of reaction is easy to be easy to control, and reaction condition is gentle, need not to increase the reaction temperature of pressure and Tai Gao, is convenient to suitability for industrialized production.(3) do not use organic crosslinking agent, avoided the pollution of toxic reagent; Used reaction reagent cheaply is easy to get, nontoxic.(4) the reaction products obtained therefrom is the fibrous sorbing material that carries iron.Fiber adsorbing material is compared with graininess or spherical sorbing material, and it is big to have specific area, and circulating resistance is little, and mechanical strength is good, and wash-out regeneration easily can be processed into various ways advantages such as (fibre bundle, nonwoven, fabrics etc.).(5) contain the hydroxide of more amorphous state iron in this material, have more activated adoption site, have stronger adsorption capacity for the arsenious acid pollutant in the water body, saturated capacity is 13 ~ 25 mg/g fibers.(6) this material stable performance in air, store method that need not be special, the pH that can not influence water body during use changes.
Description of drawings:
Fig. 1 carries the XRD spectrum contrast of iron cotton fibre material and raw material degreasing cotton fiber for the present invention.Wherein curve 1 is for carrying the iron cotton fiber; Curve 2 is former degreasing cotton fiber.
Fig. 2 carries the microphotograph (* 400) of iron cotton fibre material and raw material degreasing cotton fiber for the present invention.Wherein a figure is former degreasing cotton fiber; B figure carries the iron cotton fiber.
Fig. 3 handles the adsorption curve of arsenic (III) concentration and the processing water yield in the water outlet of back for carry the iron cotton fibre material through the present invention.
Fig. 4 handles the adsorption curve of arsenic (III) concentration and the processing water yield in the water outlet of back for carry the iron cotton fibre material through the present invention.
The specific embodiment
For better the present invention being elaborated, it is following to lift embodiment:
The 6g degreasing cotton fiber is immersed in the ferric chloride solution of 100mL5%, is warming up to 30 ℃, after 2 hours, stir the sodium hydroxide solution 105mL that dropwise adds 1M down, add speed controlling at 1ml/min.When the pH of solution value rises to 4, stop the adding of NaOH, topple over and solution, water clean fiber for several times after, repeat the adition process 6 times of above-mentioned NaOH.After carrying the iron end, left standstill 5 hours, take out then, water is washed till neutrality, in 45 ℃ baking oven, dries, the back fiber weightening finish 27.8% of weighing.Its XRD spectrum and microphotograph are respectively shown in accompanying drawing 1 and accompanying drawing 2.As can beappreciated from fig. 1, the iron that carries in the iron fiber exists with unbodied hydroxide form; As can beappreciated from fig. 2, absorbent cotton carries after the iron, still keeps fibrillar morphology.
The 350g degreasing cotton fiber is immersed in the ferrum sulfuricum oxydatum solutum of 2000mL 10%, is warming up to 25 ℃, after 3 hours, stir sodium hydroxide solution 2050 mL that dropwise add 0.5M down, add speed controlling at 20ml/min.When the pH of solution value rises to 4, stop the adding of NaOH, topple over and solution, water clean fiber for several times after, repeat the adition process 6 times of above-mentioned NaOH.After carrying the iron end, left standstill 5 hours, take out then, water is washed till neutrality, in 60 ℃ baking oven, dries, the back fiber weightening finish 16.9% of weighing.Its XRD spectrum and microphotograph such as embodiment 1.
Application examples 1
Take by weighing the fibrous material 0.1g that makes among the embodiment 1; Put into 50ml and use the water sample of the arsenic concentration of sodium arsenite preparation as 100mg/L; In 25 ℃ of vibration absorption 12 hours, the arsenic concentration that records in the solution was reduced to 50.6mg/L, and calculating this fibrous material is the 24.7mg/g fiber to the adsorbance of arsenic.
Application examples 2
Take by weighing the fibrous material 0.1g that makes among the embodiment 2; Put into 50ml and use the water sample of the arsenic concentration of sodium arsenite preparation as 100mg/L; In 25 ℃ of vibration absorption 12 hours, the arsenic concentration that records in the solution was reduced to 59.3mg/L, and calculating this fibrous material is the 20.3mg/g fiber to the adsorbance of arsenic.
Application examples 3
Take by weighing the fibrous material 2g that makes among the embodiment 1; Load highly to 10cm, diameter are the adsorption column of 1cm, with arsenic (III) concentration be the water sample of 1mg/L with the flow velocity of 1mL/min through adsorption column, water inlet pH=6.96; The arsenic concentration of monitoring water outlet; When the processing water yield was in 40.3L, the arsenic concentration of water outlet was lower than 50mg/L, water outlet pH=6.93.Adsorption curve such as accompanying drawing 3.And, show that this year, iron adsorbent carried the iron form stable through detecting iron concentration in the Inlet and outlet water.
Application examples 4
Take by weighing the fibrous material 2g that makes among the embodiment 2; Load highly to 10cm, diameter are the adsorption column of 1cm, with arsenic (III) concentration be the water sample of 1mg/L with the flow velocity of 1mL/min through adsorption column, water inlet pH=6.96; The arsenic concentration of monitoring water outlet; When the processing water yield was in 35.8L, the arsenic concentration of water outlet was lower than 50mg/L, water outlet pH=6.92.Adsorption curve such as accompanying drawing 4.And, show that this year, iron adsorbent carried the iron form stable through detecting iron concentration in the Inlet and outlet water.
Claims (5)
1. one kind carries the iron cotton fibre material, it is characterized in that: as basic skeleton, contain the iron hydroxide that exists with amorphous state with degreasing cotton fiber, and kept the fibrous form of degreasing cotton fiber; And be prepared from: with the degreasing cotton fiber washing, be immersed in mass percent and be 2% ~ 10%, temperature is in 10 ~ 50 ℃ the ferric iron aqueous solution, after 1 ~ 3 hour through following steps; Stir; The aqueous slkali that dropwise adds 0.5 ~ 2M, trivalent iron salt through disperse, hydrolysis is written into absorbent cotton, in air, leave standstill 3 ~ 8 hours after; Water is washed till neutrality, in 30 ~ 80 ℃ of oven dry.
2. as claimed in claim 1 year iron cotton fibre material is characterized in that: used absorbent cotton filament length is 3 ~ 7 cm, and the tension brute force is 0.021 ~ 0.054N.
3. according to claim 1 or claim 2 the preparation method of carrying the iron cotton fibre material is characterized in that: realizes through following steps: degreasing cotton fiber is washed, be immersed in mass percent and be 2% ~ 10%, temperature is in 10 ~ 50 ℃ the ferric iron aqueous solution; After 1 ~ 3 hour, stir, dropwise add the aqueous slkali of 0.5 ~ 2M; Trivalent iron salt is written into absorbent cotton through dispersion, hydrolysis; After in air, leaving standstill 3 ~ 8 hours, water is washed till neutrality, in 30 ~ 80 ℃ of oven dry.
4. the preparation method of as claimed in claim 3 year iron cotton fibre material is characterized in that: the ferric iron aqueous solution is 1:3 with aqueous slkali maximum volume ratio.
5. the preparation method of as claimed in claim 3 year iron cotton fibre material is characterized in that: the fiber weightening finish of oven dry back is controlled at 10% ~ 40%.
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| CN104084140B (en) * | 2014-07-04 | 2016-08-24 | 淮海工学院 | Heavy metal copper ion adsorbent and preparation method thereof in a kind of high-salt wastewater |
| CN105344332A (en) * | 2015-11-04 | 2016-02-24 | 苏州书瑞环保科技有限公司 | Water treatment arsenic adsorption material and preparation method thereof |
| CN105797782A (en) * | 2016-03-11 | 2016-07-27 | 河南师范大学 | Iron-loaded cotton fiber-doped nanometer titanium dioxide composite fiber material and preparation method thereof |
| CN109231280A (en) * | 2018-10-12 | 2019-01-18 | 山东理工大学 | A kind of preparation method of rice-shaped di-iron trioxide composite cotton fabric carbon fibre material |
| CN115400502A (en) * | 2022-09-20 | 2022-11-29 | 西安兴晟生态环境有限公司 | SPF fiber filter cake material for direct cleaning filter and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1589959A (en) * | 2003-08-28 | 2005-03-09 | 王军锋 | Preparation method of high selectivity iron carrier ligand exchange cotton fiber adsorbent |
| CN1593745A (en) * | 2004-07-05 | 2005-03-16 | 南开大学 | Ferrum carried spherical cellulose adsorbent, preparation and application thereof |
| CN101569854A (en) * | 2009-06-05 | 2009-11-04 | 河南省科学院化学研究所有限公司 | Arsenic adsorbing fiber and synthesizing method thereof |
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| JP4420634B2 (en) * | 2003-08-19 | 2010-02-24 | 日鉄環境エンジニアリング株式会社 | Treatment method of acid mine wastewater containing arsenic and iron |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1589959A (en) * | 2003-08-28 | 2005-03-09 | 王军锋 | Preparation method of high selectivity iron carrier ligand exchange cotton fiber adsorbent |
| CN1593745A (en) * | 2004-07-05 | 2005-03-16 | 南开大学 | Ferrum carried spherical cellulose adsorbent, preparation and application thereof |
| CN101569854A (en) * | 2009-06-05 | 2009-11-04 | 河南省科学院化学研究所有限公司 | Arsenic adsorbing fiber and synthesizing method thereof |
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| JP特开2005-58955A 2005.03.10 |
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