CN102872821A - Composite adsorbing material for removing vanadium ions in natural water and preparation method thereof - Google Patents
Composite adsorbing material for removing vanadium ions in natural water and preparation method thereof Download PDFInfo
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- CN102872821A CN102872821A CN2012103221647A CN201210322164A CN102872821A CN 102872821 A CN102872821 A CN 102872821A CN 2012103221647 A CN2012103221647 A CN 2012103221647A CN 201210322164 A CN201210322164 A CN 201210322164A CN 102872821 A CN102872821 A CN 102872821A
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Abstract
The invention belongs to the field of water treatment in environmental-protection industry, and particularly relates to a preparation method of novel composite adsorbing material prepared by loading crosslinked chitosan on modified apocynum venetum short fibers for removing lithium ions in natural water. The preparation method comprises the steps as follows: preparing crosslinked chitosan through chitosan, epichlorohydrin and sodium hydroxide; then carrying out basification modification to apocynum venetum fibers so as to obtain the modified apocynum venetum short fibers; uniformly mixing to compositing the crosslinked chitosan and the modified apocynum venetum short fibers; and finally precipitating, washing, filtering, centrifuging and drying in the air to obtain the composite adsorbing material. The composite adsorbing material provided by the invention has the characteristics that the selective adsorption property on the vanadium ions is efficient, the regenerating and recycling effects are good, the operation is simple, no secondary pollution is caused, the price is low, the efficiency is high, and the like. The preparation method provided by the invention is simple in technology, low in cost, high in efficiency and beneficial for environmental protection, and has high economic and social benefits in the field of water treatment.
Description
Technical field
The present invention relates to a kind of composite adsorbing material of removing vanadium ion in the natural water body and preparation method thereof, be specifically related to utilize cross-linked chitosan to load on a kind of novel material that makes on the bluish dogbane modified short fiber, belong to the purifying water process field.
Background technology
Vanadium is a kind of dystectic rare metal, is widely used in metallurgy, chemistry, aircraft and auto manufacturing, national defense industry and other field.Vanadium also is one of trace element of needed by human, but excessive vanadium is to the toxic effect of human body, and its toxicity increases with valent rising.Therefore, the vanadium in analysis, the research environment sample, tool is of great significance.
At present, mainly contain extraction and ion-exchange for the method for removing the natural water body vanadium ion.The vanadium extraction effect of solvent extraction is better, but extraction conditions is harsh, fluctuation of service and easily form secondary pollution: the ion exchange extraction vanadium method starts to walk early abroad, usually first vanadium is changed into the water-soluble vanadium ion that contains, then adopt different ion-exchangers according to different material, with ion exchange resin generation adsorption reaction, vanadium is adsorbed on the ion exchange resin, through wash-out vanadium is changed in the eluent again.Ion-exchange is as a kind of new technology of Vanadium Concentrationin, and its advantages of good adsorption effect is rising, but serious deficiency is being arranged aspect the recycling of its material.In sum, these two kinds of methods can not recycling and produce and very large defective is arranged aspect the secondary pollution at material.
The present invention is that a kind of effectively and economic composite adsorbing material the present invention compares with above-mentioned two kinds of methods, have the material regeneration utilization rate large, can be recycled, the characteristics such as non-secondary pollution.Realize the comprehensive utilization of house refuse, protected environment, widened the range of choice of composite in the water adsorption treatment process, realized the resource of discarded object, had good Social benefit and economic benefit.
Summary of the invention
The objective of the invention is provides a kind of composite adsorbing material of removing vanadium ion in the natural water body and preparation method thereof in order to overcome existing technology in the deficiency aspect material regeneration utilization and the secondary pollution.The present invention is a kind of novel composite adsorbing material, has that adsorption efficiency is high, simple to operate, cost is low, and recovery utilization rate is large, and can regenerate the characteristics such as non-secondary pollution.
The objective of the invention is to be achieved through the following technical solutions:
1, raw material screening
Cross-linked chitosan and bluish dogbane short fiber reaction preparation composite: (1) skeleton raw material: shitosan, epoxychloropropane: the second raw material is NaOH.(2) the 3rd raw materials are the bluish dogbane short fiber that apocynum fibre alkali puffing and modifying becomes;
2, composite adsorbing material preparation
Get cross-linked chitosan 15～20g, mix with the modified short fiber that makes and to be positioned in the container, to wherein adding 5～10ml distilled water, heated at constant temperature and stirring under 50～70 ℃ of conditions, take out, repeatedly wash 3～5 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
Principle of the present invention: cross-linked chitosan is a kind of cancellated high molecular polymer that has, and thereby its surperficial amino group provides lone pair electrons to forming the purpose that complex compound reaches absorption with vanadium ion by chemisorbed, the short fiber of puffing and modifying then provides huge specific area for adsorption reaction, so this composite adsorbing material Adsorption vanadium ion has efficient absorption property.
Application process of the present invention: the vanadium ion solution 50mL that gets 20mg/L regulates after the pH value is 4.0 with ammoniacal liquor, change in the tool plug conical flask that 50mg cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material is housed, put the 2h that vibrates on the shaking table, filter, record that vanadium ion concentration is less than 300ug in the water, clearance of the present invention reaches 99.9%.
The invention has the beneficial effects as follows:
(1) cross-linked chitosan is a kind of cancellated high molecular polymer that has, and it all has goodish absorption property in acidity and alkaline solution;
(2) the present invention takes full advantage of industrial waste, and raw material is easy to get, low price, and the preparation method is simple, is used for water treatment, and 5～10min can reach adsorption equilibrium, and adsorbance is large;
(3) disposal cost of the present invention is cheap, and waste residue can acidifiedly be processed, the recyclable recycling of material.
The specific embodiment
The objective of the invention is to be achieved through the following technical solutions:
1, takes by weighing in the acetic acid solution that 4～6g shitosan is dissolved in 250～300mL 1%, slowly add 4～6mL epoxychloropropane under the vigorous stirring, drip gradually the oxygen sodium oxide molybdena of 30～40mL5%, continue reaction 12～15h, until generation white solid, behind the suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing.Dry, mill, for subsequent use after the screening;
2, (the 8%owf pectase is processed 3～4h), soda boilings at normal temperatures, and (sodium hydroxide solution of 8g/L makes apocynum fibre in 80～90 ℃ of lower processing 0.5～1h), secondary soda boiling (sodium hydroxide solution of 20g/L is at 80～90 ℃ of lower 1-2h of processing) 3～5 50～60 ℃ of oven dry of after washing by the pectase processing with bluish dogbane raw ramie skin.(length≤20mm) carry out the alkali puffing and modifying obtains modification bluish dogbane short fiber by washing, oven dry at last to apocynum fibre by the oxygen sodium hydroxide solution again;
3, get cross-linked chitosan 15～20g, mix with the modified short fiber that makes and to be positioned in the container, to wherein adding 5～10ml distilled water, heated at constant temperature and stirring under 50～70 ℃ of conditions, take out, repeatedly wash 3～5 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
[0011] example 1
Take by weighing in the acetic acid solution that the 6g shitosan is dissolved in 300mL 1%, slowly add the 6mL epoxychloropropane under the vigorous stirring, drip gradually the NaOH of 40mL5%, continue reaction 15h, until generate white solid, behind the suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing.Dry, mill, for subsequent use after the screening.Bluish dogbane raw ramie skin is made apocynum fibre by pectase processing (the 8%owf pectase is processed 4h at normal temperatures), a soda boiling (sodium hydroxide solution of 8g/L is at 90 ℃ of lower 1h of processing), secondary soda boiling (sodium hydroxide solution of 20g/L is at 90 ℃ of lower 2h that process) 560 ℃ of oven dry of after washing.(length≤20mm) carry out the alkali puffing and modifying obtains modification bluish dogbane short fiber by washing, oven dry at last to apocynum fibre by sodium hydroxide solution again.Get cross-linked chitosan 20g, mix being positioned in the container with the modified short fiber that makes, to wherein adding 10ml distilled water, heated at constant temperature and stirring under 70 ℃ of conditions, take out, repeatedly wash 5 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
Example 2
Take by weighing in the acetic acid solution that the 4g shitosan is dissolved in 250mL1%, slowly add the 4mL epoxychloropropane under the vigorous stirring, drip gradually the NaOH of 30mL5%, continue reaction 12h, until generate white solid, behind the suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing.Dry, mill, for subsequent use after the screening.Bluish dogbane raw ramie skin is made apocynum fibre by pectase processing (the 8%owf pectase is processed 3h at normal temperatures), a soda boiling (sodium hydroxide solution of 8g/L is at 80～90 ℃ of lower 0.5h of processing), secondary soda boiling (sodium hydroxide solution of 20g/L is at 80 ℃ of lower 1h that process) 3 50 ℃ of oven dry of after washing.(length≤20mm) carry out the alkali puffing and modifying obtains modification bluish dogbane short fiber by washing, oven dry at last to apocynum fibre by sodium hydroxide solution again.Get cross-linked chitosan 15g, mix being positioned in the container with the modified short fiber that makes, to wherein adding 5ml distilled water, heated at constant temperature and stirring under 50 ℃ of conditions, take out, repeatedly wash 3 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
Example 3
Take by weighing in the acetic acid solution that the 5g shitosan is dissolved in 270mL1%, slowly add the 5mL epoxychloropropane under the vigorous stirring, drip gradually the NaOH of 35mL5%, continue reaction 14h, until generate white solid, behind the suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing.Dry, mill, for subsequent use after the screening.Bluish dogbane raw ramie skin is made apocynum fibre by pectase processing (the 8%owf pectase is processed 3.5h at normal temperatures), a soda boiling (sodium hydroxide solution of 8g/L is at 85 ℃ of lower 1h of processing), secondary soda boiling (sodium hydroxide solution of 20g/L is at 85 ℃ of lower 1h that process) 4 55 ℃ of oven dry of after washing.(length≤20mm) carry out the alkali puffing and modifying obtains modification bluish dogbane short fiber by washing, oven dry at last to apocynum fibre by sodium hydroxide solution again.Get cross-linked chitosan 17g, mix being positioned in the container with the modified fibre that makes, to wherein adding 8ml distilled water, heated at constant temperature and stirring under 60 ℃ of conditions, take out, repeatedly wash 4 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
Claims (7)
1. composite adsorbing material of removing vanadium ion in the natural water body, it is characterized in that: this composite adsorbing material reacts take shitosan, epoxychloropropane and NaOH raw material as skeleton makes cross-linked chitosan, again take alkali puffing and modifying bluish dogbane short fiber as the inclusion organic matter.
2. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 1, the preparation method who it is characterized in that cross-linked chitosan: take by weighing in the acetic acid solution that 4～6g shitosan is dissolved in 250～300mLl%, slowly add 4～6mL epoxychloropropane under the vigorous stirring, drip gradually the NaOH of 30～40mL5%, continue reaction 12～15h, until generation white solid, behind the suction filtration, wash with water to neutrality, again with a small amount of acetone rinsing, dry, mill, for subsequent use after the screening.
3. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 1, the preparation method who it is characterized in that bluish dogbane short fiber alkali puffing and modifying: bluish dogbane raw ramie skin is made apocynum fibre by pectase processing, a soda boiling, 3～5 50～60 ℃ of oven dry of secondary soda boiling after washing, (length≤20mm) is carried out the alkali puffing and modifying, obtains modification and spreads out short fiber by washing, flood are dried at last to apocynum fibre by sodium hydroxide solution again.
4. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 3 is characterized in that: it is to process at normal temperatures 3～4h with the 8%owf pectase that described pectase is processed.
5. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 3 is characterized in that: a described soda boiling is that the dark liquid of NaOH with 8g/L is at 80～90 ℃ of lower 0.5～1h of processing.
6. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 3 is characterized in that: described secondary soda boiling is that sodium hydroxide solution with 20g/L is at 80～90 ℃ of lower 1～2h of processing.
7. a kind of composite adsorbing material of removing vanadium ion in the natural water body according to claim 1, the complex method that it is characterized in that cross-linked chitosan and modified short fiber: get cross-linked chitosan 15～20g, mix with the modified short fiber that makes in the claim 3 and to be positioned in the container, to wherein adding 5～10ml distilled water, heated at constant temperature and stirring under 50～70 ℃ of conditions, take out, repeatedly wash 3～5 times with deionized water, can make cross-linked chitosan-bluish dogbane modified short fiber composite adsorbing material.
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| CN104907050A (en) * | 2015-05-13 | 2015-09-16 | 中国广州分析测试中心 | Composite material with enrichment function of titanium and vanadium in water and preparation method therefor |
| CN107552015A (en) * | 2017-10-31 | 2018-01-09 | 成都先进金属材料产业技术研究院有限公司 | A kind of modified mangosteen shell and the method using vanadium in its reduction water body |
| CN108408864A (en) * | 2018-05-09 | 2018-08-17 | 东莞市石鼓污水处理有限公司 | A kind of sewage disposal precipitating reagent |
| CN108483677A (en) * | 2018-05-09 | 2018-09-04 | 东莞市石鼓污水处理有限公司 | A kind of flocculant for clarifying sewage |
| CN108483607A (en) * | 2018-05-09 | 2018-09-04 | 东莞市石鼓污水处理有限公司 | A kind of sewage treatment flocculating agent |
| CN108940220A (en) * | 2018-07-26 | 2018-12-07 | 赣州市翔义科技有限公司 | A kind of modification of chitosan material and preparation method for the sewage treatment containing vanadium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104907050A (en) * | 2015-05-13 | 2015-09-16 | 中国广州分析测试中心 | Composite material with enrichment function of titanium and vanadium in water and preparation method therefor |
| CN107552015A (en) * | 2017-10-31 | 2018-01-09 | 成都先进金属材料产业技术研究院有限公司 | A kind of modified mangosteen shell and the method using vanadium in its reduction water body |
| CN107552015B (en) * | 2017-10-31 | 2020-11-10 | 成都先进金属材料产业技术研究院有限公司 | Modified mangosteen shell and method for reducing vanadium in water body by using same |
| CN108408864A (en) * | 2018-05-09 | 2018-08-17 | 东莞市石鼓污水处理有限公司 | A kind of sewage disposal precipitating reagent |
| CN108483677A (en) * | 2018-05-09 | 2018-09-04 | 东莞市石鼓污水处理有限公司 | A kind of flocculant for clarifying sewage |
| CN108483607A (en) * | 2018-05-09 | 2018-09-04 | 东莞市石鼓污水处理有限公司 | A kind of sewage treatment flocculating agent |
| CN108940220A (en) * | 2018-07-26 | 2018-12-07 | 赣州市翔义科技有限公司 | A kind of modification of chitosan material and preparation method for the sewage treatment containing vanadium |
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Application publication date: 20130116 |