CN102872818A - Composite adsorbing material for removing zinc ions in natural water and preparation method thereof - Google Patents
Composite adsorbing material for removing zinc ions in natural water and preparation method thereof Download PDFInfo
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- CN102872818A CN102872818A CN2012103221454A CN201210322145A CN102872818A CN 102872818 A CN102872818 A CN 102872818A CN 2012103221454 A CN2012103221454 A CN 2012103221454A CN 201210322145 A CN201210322145 A CN 201210322145A CN 102872818 A CN102872818 A CN 102872818A
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Abstract
The invention discloses a composite adsorbing material for removing zinc ions in natural water and a preparation method of the composite adsorbing material. The specific method is as follows: combining the decolored and modified orange peel and insoluble starch xanthate, and obtaining a starch xanthate and orange peel composite adsorbing material; and after the preparation, feeding 10g of the composite adsorbing material into the waste water with volume of 300mL and zinc ion concentration of 100mg/L, finishing the preparation after adjusting the pH (Potential Of Hydrogen) value to 6 to 8, standing and adsorbing for 2 to 3h, wherein the concentration of the zinc ions in the waste water is measured to be below 1mg/L, so that the waste water reaches the secondary national standard of surface water. The composite adsorbing material for removing the zinc ions in the natural water, provided by the invention, has the following advantages that: 10 to 15% of hydrochloric acid is added into an adsorbing agent after the adsorption, so that the zinc ions can be recovered and adsorbed and the adsorbing material can be recycled. The composite adsorbing material for removing the zinc ions in the natural water, provided by the invention, has the characteristics of low cost, simplicity in technology, quickness in reaction, high treatment efficiency, wide application range, and the like.
Description
Technical field
The present invention is a kind of composite adsorbing material and preparation thereof of removing zinc ion in the natural water body, is specifically related to be rich in the processing of the sewage of zinc ion, belongs to the dirty water decontamination handles field in the environment.
Background technology
Zinc is a kind of heavy metal resources, is widely used among modern industry production such as smelting, pharmacy and the food service industry that a large amount of zinc-containing waters is to the environmental emission serious harm mankind's health in process of production.Zinc is indispensable trace element in the growing process, and it is the constituent of many synzyme in the plant, and the limited promotion photosynthesis of energy participates in the synthetic of auxin and protein.Zinc is the indispensable element of health, it extensively is present in human muscle and the bone, participate in the metabolic process of nucleic acid protein, can promote the normal development of skin, a bone sexual organ, keep the digestion and metabolism activity, but content is very little, if too high at people's in-vivo content, will suppress phagocytal activity and sterilizing power, thus reduce human body immunologic function, resistance is weakened.Therefore zinc ion is removed or extracted to research from the natural water body kind, on the one hand can environmental contamination reduction, saving water resource; On the other hand again can playback comprehensive utilization zinc resource.
At present, a lot of for the removal method of zinc ion both at home and abroad, comprise that chemical method, ion-exchange, absorption method, hyperfiltration, electroosmose process and solvent extraction put etc.Be chemical method in industrial generally employing method, yet the chemical method cost is high, easily produces secondary pollution.Ion-exchange has that treating capacity is large, effluent quality reaches well the advantages such as recyclable water, but resin vulnerable to pollution or oxidation deactivation.Although the employed adsorbent raw material sources of absorption method are wide, easy to manufacture, inexpensive, service life is short.Hyperfiltration has plurality of advantages, and such as small investment, floor space is little, operation control aspect is simple, but for avoiding impurities accumulation, be used in combination with ion-exchange.Electroosmose process has certain limit for pending concentration of metal ions, can not process thoroughly.The extractant of solvent extraction is expensive, generally without this method.Thereby a kind of advanced composite material (ACM) of need exploitation comes the zinc ion in more effective processing natural water body.
The insoluble starch xanthate is the high crosslinked starch that the starch crosslinking agent forms under alkali condition, what form through xanthogenation, is a kind of novel efficient adsorption heavy metal material.
The main component of orange skin is cellulose.Fine little plain molecule contains many hydrophilic oh groups, it is a kind of ionomer of fibrous, multiple capillary, has the large characteristic of porous and specific surface area, therefore has affine adsorptivity, but adsorption capacity is not strong, must make by chemical modification to have stronger or more hydrophilic radical, become well behaved sorbing material.
Summary of the invention
The shortcomings such as the present invention is take starch xanthate-orange skin as composite adsorbing material, and is short for the employed adsorbent of the absorption method life-span commonly used, that operating cost is high provide a kind of composite adsorbing material of removing the zinc ion in the natural water body and preparation method thereof.Composite adsorbing material of the present invention still can reuse after the alkali pickling is washed, thereby has the advantage that cost is low, investment is little.In addition, starch and orange skin all easily obtain, process conveniently, and whole course of reaction is stable, and controllability is strong, can not cause secondary pollution etc.
Technical scheme of the present invention is:
(1) get first common starch 20～30g, be positioned in the container, add the N of 3～5ml, the inside alkene acid amides of N '-di-2-ethylhexylphosphine oxide, the sodium hydroxide solution 40～50mL of adding 20% continues stirring reaction 10～12h behind stirring 10～15min;
(2) add respectively again 5% hydrochloric acid 10mL, 5～7ml carbon disulfide in the container, behind stirring reaction 1～2h, modification orange skin is joined in the starch solution of handling well, place constant-temperature table, it is 20～30 ℃ in temperature, 30min is left standstill after fully vibrating and contacting 2h in the condition countryside of 200/min;
(3) filter at last, be used for ionized water washing 2～3 times, 20～30 ℃ of lower oven dry, make starch xanthate-orange skin composite adsorbing material.
The method of modifying of described orange skin is:
(1) at first gets fresh orange skin 80～100g, use deionized water rinsing 2～3 times, 50～60 ℃ of lower oven dry, pulverize, cross 50 mesh sieves;
(2) get again orange skin 30～50g after the above-mentioned processing, join in the hydrogenperoxide steam generator of 100mL mass fraction 9%, jointly place the micro-wave oven microwave heating treatment 1min of 480w;
(3) take out at last, filter, the citric acid with 10～20% washes 2～4 times repeatedly, 40～50 ℃ of lower oven dry, makes modification orange skin.
Described N, N '-methylene-bisacrylamide make starch reaction be called highly cross-linked crosslinked starch under alkali condition as crosslinking agent, crosslinked starch again with carbon disulfide generation xanthan acidification response, generate the insoluble starch xanthate.
Principle of the present invention is: modification orange skin porous, specific area from now on is large, and good absorption property is arranged, and the insoluble starch xanthate adheres on it, can form insoluble complex compound by complexing with zinc ion, is adsorbed in the hole of orange skin.Effectively process zinc ion in the natural water body by this principle.
Concrete application process of the present invention is: get the composite adsorbing material 100g for preparing, rendering to volume is that 300mL, zinc ion concentration are in the sewage of 100mg/L, and adjusting pH value is 6～8, unexpectedly puts and takes out composite adsorbing material after adsorbing 2～3h, finishes absorption.Add 10～15% hydrochloric acid in the adsorbent after use again, i.e. the recyclable zinc ion that is adsorbed onto.The concentration that records the zinc ion in the sewage is below the 1mg/L, reaches national surface water quality secondary standard.
Beneficial effect of the present invention is:
(1) composite adsorbing material of the present invention has significant economic benefit for the processing of zinc ion in the sewage, and on the one hand, material is general easily to be obtained, and material price is cheap; On the other hand, in use, the pharmaceutical quantities of input is few, and effect is remarkable;
(2) after the absorption of this kind composite adsorbing material is finished, can carry out acidleach to material and process, the zinc ion that recoverable is adsorbed onto, sorbing material also can drop into re-using again, have really realized the environmental protection processing;
(3) the present invention also have simple to operate, be swift in response, the advantage such as treatment effeciency is high, the scope of application of pH is 6～8, and is applied widely.
The specific embodiment
The technical solution used in the present invention is as follows:
At first get fresh orange skin 80～100g, use deionized water rinsing 2～3 times, 50～60 ℃ of lower oven dry, pulverize, cross 50 mesh sieves; Get again the orange skin 30～50g after the above-mentioned processing, add in the hydrogenperoxide steam generator of 100mL mass fraction 9%, place the micro-wave oven microwave heating treatment 1min of 480w therebetween; Take out at last, filter, the citric acid with 10～20% washes 2～4 times repeatedly, 40～50 ℃ of lower oven dry, makes modification orange skin;
Simultaneously, get common starch 20～30g, be positioned in the container, add the N of 3～5mL, N '-methylene-bisacrylamide, the sodium hydroxide solution 40～50mL of adding 20% continues stirring reaction 10～12h behind stirring 10～15min; Add respectively again 5% hydrochloric acid 10mL, 5～7mL carbon disulfide in the container, behind stirring reaction 1～2h, modification orange skin is joined in the starch solution of handling well, place constant-temperature table, be 20～30 ℃ in temperature, fully behind the vibration contact 2h, leave standstill 30min under the condition of 200r/min; Filter at last, with deionized water washing 2～3 times, 20～30 ℃ of lower oven dry, make starch xanthate-orange skin composite adsorbing material.
Example 1
At first get fresh orange skin 80g, use deionized water rinsing 2 times, 50 ℃ of lower oven dry, pulverize, cross 50 mesh sieves; Get the orange skin 30g after the above-mentioned processing again, join in the hydrogenperoxide steam generator of 100mL mass fraction 9%, it is with the micro-wave oven microwave heating treatment 1min that places 480w; Take out at last, filter, the citric acid with 10% washes 2 times repeatedly, 40 ℃ of lower oven dry, makes modification orange skin;
Simultaneously, get common starch 20g, be positioned in the container, add the N of 3ml, N '-methylene-bisacrylamide, the sodium hydroxide solution 40mL of adding 20% continues stirring reaction 10h behind the stirring 10min; Add respectively again 5% hydrochloric acid 100mL, 5ml carbon disulfide in the container, behind the stirring reaction 1h, modification orange skin is joined in the starch solution of handling well, place constant-temperature table, be 20 ℃ in temperature, fully behind the vibration contact 2h, leave standstill 30min under the condition of 200r/min; Filter at last, with deionized water washing 2 times, 20 ℃ of lower oven dry, make starch xanthate-orange skin composite adsorbing material.
Get the composite adsorbing material 10g for preparing in the example 1, rendering to volume is that 300mL, zinc ion concentration are in the sewage of 100mg/L, adjusting the pH value is 6, take out composite adsorbing material behind the standing adsorption 2h, the concentration that records the zinc ion in the sewage is 0.99mg/L, reaches national surface water quality secondary standard quality secondary standard.
Example 2
At first get fresh orange skin 90g, use deionized water rinsing 3 times, 55 ℃ of lower oven dry, pulverize, cross 50 mesh sieves; Get again the orange skin 40g after the above-mentioned processing, join in the hydrogenperoxide steam generator of 100mL mass fraction 9%, jointly place the little heat treated 1min of micro-wave oven of 480w; Take out at last, filter, the citric acid with 15% washes 3 times repeatedly, 45 ℃ of lower oven dry, makes modification orange skin;
Simultaneously, get common starch 25g, be positioned in the container, add the N of 4ml, N '-methylene-bisacrylamide, the sodium hydroxide solution 45mL of adding 20% continues stirring reaction 11h behind the stirring 15min; Add respectively again 5% hydrochloric acid 10mL, 6mL carbon disulfide in the container, behind the stirring reaction 1.5h, modification orange skin is joined in the starch solution of handling well, place constant-temperature table, be 25 ℃ in temperature, fully behind the vibration contact 2h, leave standstill 30min under the condition of 200r/min; Filter at last, with deionized water washing 3 times, 25 ℃ of lower oven dry, make the compound absorption material of starch xanthate-orange skin.
Get the composite adsorbing material 10g for preparing in the example 2, rendering to volume is that 300mL, zinc ion concentration are in the sewage of 100mg/L, adjusting the pH value is 7, take out composite adsorbing material behind the standing adsorption 3h, the concentration that records the zinc ion in the sewage is 0.76mg/L, reaches national surface water quality secondary standard.
Example 3
At first get fresh orange skin 100g, use deionized water rinsing 3 times, 60 ℃ of lower oven dry, pulverize, cross 50 mesh sieves; Get again the orange skin 50g after the above-mentioned processing, join in the peroxide solution of 100mL mass fraction 9%, jointly place the micro-wave oven microwave heating treatment 1min of 480w; Take out at last, filter, the citric acid with 20% washes 4 times repeatedly, 50 ℃ of lower oven dry, makes modification orange skin;
Simultaneously, get common starch 30g, be positioned in the container, add the N of 5ml, N '-methylene-bisacrylamide, the sodium hydroxide solution 50mL of adding 20% continues stirring reaction 12h behind the stirring 15min; Add respectively again 5% hydrochloric acid 10mL, 7mL carbon disulfide in the container, behind the stirring reaction 2h, modification orange skin is joined in the starch solution of handling well, place constant-temperature table, be 30 ℃ in temperature, fully behind the vibration contact 2h, leave standstill 30min under the condition of 200r/min; Filter at last, with deionized water washing 3 times, 30 ℃ of lower oven dry, make starch xanthate-orange skin composite adsorbing material.
Get the composite adsorbing material 10g for preparing in the example 3, rendering to volume is that 300mL, zinc ion concentration are in the sewage of 100mg/L, adjusting the pH value is 8, take out composite adsorbing material after leaving standstill absorption 3h, the concentration that records the zinc ion in the sewage is 0.23mg/L, reaches national surface water quality secondary standard.
Claims (4)
1. composite adsorbing material of removing zinc ion in the natural water body and preparation method thereof is characterized in that: orange skin and the insoluble starch xanthate of composite adsorbing material after by modification is prepared from.
2. a kind of composite adsorbing material of removing zinc ion in the natural water body according to claim 1 and preparation method thereof is characterized in that the method for modifying of described orange skin is:
(1) at first gets fresh orange skin 80～100g, use deionized water rinsing 2～3 times, 50～60 ℃ of lower oven dry, pulverize, cross 50 mesh sieves;
(2) get again orange skin 30～50g after the above-mentioned processing, join in the hydrogenperoxide steam generator of 100mL mass fraction 9%, jointly place the micro-wave oven microwave heating treatment 1min of 480w;
(3) take out at last, filter, the citric acid with 10～20% washes 2～4 times repeatedly, 40～50 ℃ of lower oven dry, makes modification orange skin.
3. a kind of composite adsorbing material of removing zinc ion in the natural water body according to claim 1 and preparation method thereof is characterized in that the carrying method of described orange skin load starch xanthate is:
(1) get first common starch 20～30g, be positioned in the container, add the N of 3～5ml, N '-methylene-bisacrylamide, the sodium hydroxide solution 40～50mL of adding 20% behind stirring 10～15min, continue stirring reaction 10～12h:
(2) add respectively again 5% hydrochloric acid 10mL, 5～7ml carbon disulfide in the container, behind stirring reaction 1～2h, modification orange skin in the claim 2 is joined in the starch solution of handling well, place constant-temperature table, it is 20～30 ℃ in temperature, after fully vibration contacts 2h under the condition of 200r/min, leave standstill 30min;
(3) filter at last, with deionized water washing 2～3 times, 20～30 ℃ of lower oven dry, make starch xanthate-orange skin composite adsorbing material.
4. a kind of composite adsorbing material of removing zinc ion in the natural water body according to claim 3 and preparation method thereof, it is characterized in that: N, N '-methylene-bisacrylamide is as crosslinking agent, under alkali condition, make starch reaction be called highly cross-linked crosslinked starch, with carbon disulfide generation xanthan acidification response, generate the insoluble starch xanthate again.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894156A (en) * | 2014-03-06 | 2014-07-02 | 薛松晓 | Method for manufacturing heavy metal ion adsorbent by using orange peel |
| CN104556327A (en) * | 2014-12-19 | 2015-04-29 | 林昌民 | Electroplating wastewater comprehensive treating agent |
| CN106179241A (en) * | 2016-07-14 | 2016-12-07 | 胡大苇 | A kind of preparation method of the chelating agen processing heavy metal in waste water |
| CN109464984A (en) * | 2018-10-23 | 2019-03-15 | 常州大学 | A kind of oriental plant branch processing method |
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| US4455245A (en) * | 1982-02-19 | 1984-06-19 | Klein Pearl M | Flocculating reagent |
| JP2577845B2 (en) * | 1992-02-28 | 1997-02-05 | 逸郎 古澤 | Water purification material |
| CN102059099A (en) * | 2010-12-10 | 2011-05-18 | 中南大学 | Biological adsorbent for waste water treatment and preparation method thereof |
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- 2012-08-28 CN CN2012103221454A patent/CN102872818A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4455245A (en) * | 1982-02-19 | 1984-06-19 | Klein Pearl M | Flocculating reagent |
| JP2577845B2 (en) * | 1992-02-28 | 1997-02-05 | 逸郎 古澤 | Water purification material |
| CN102059099A (en) * | 2010-12-10 | 2011-05-18 | 中南大学 | Biological adsorbent for waste water treatment and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894156A (en) * | 2014-03-06 | 2014-07-02 | 薛松晓 | Method for manufacturing heavy metal ion adsorbent by using orange peel |
| CN103894156B (en) * | 2014-03-06 | 2016-02-10 | 薛松晓 | A kind of method utilizing orange peel to make adsorbent for heavy metal |
| CN104556327A (en) * | 2014-12-19 | 2015-04-29 | 林昌民 | Electroplating wastewater comprehensive treating agent |
| CN106179241A (en) * | 2016-07-14 | 2016-12-07 | 胡大苇 | A kind of preparation method of the chelating agen processing heavy metal in waste water |
| CN106179241B (en) * | 2016-07-14 | 2018-08-24 | 胡大苇 | A kind of preparation method of the chelating agent of processing heavy metal in waste water |
| CN109464984A (en) * | 2018-10-23 | 2019-03-15 | 常州大学 | A kind of oriental plant branch processing method |
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Application publication date: 20130116 |