CN105478072A - Method for preparing modified shell powder - Google Patents
Method for preparing modified shell powder Download PDFInfo
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- CN105478072A CN105478072A CN201510938663.2A CN201510938663A CN105478072A CN 105478072 A CN105478072 A CN 105478072A CN 201510938663 A CN201510938663 A CN 201510938663A CN 105478072 A CN105478072 A CN 105478072A
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- oyster shell
- shell whiting
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- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a method for preparing modified shell powder. The method comprises the following steps: a step (1) of preparing shell powder; a step (2) of preparing modified carbon nanotubes; and a step (3) of preparing modified shell powder. The shell powder formed by processing shells serves as a main raw material, the shell powder is modified through the modified carbon nanotubes, so that the heavy metal ion adsorption capability of the shell powder is greatly improved, and an effective way is provided for improving shell powder utilization rate, developing natural adsorbents and performing heavy metal ion wastewater treatment.
Description
Technical field
The present invention relates to a kind of heavy metal absorbent, especially relate to a kind of preparation method of modification oyster shell whiting.
Background technology
Along with socioeconomic development, increasing to the demand of water, but on the one hand the water resource of China is relatively very in short supply, water pollution is quite serious on the other hand, and particularly the heavy metal pollution that causes of the industry such as plating, metallurgy, pigment is startling.The technology of process effluent containing heavy metal ions has chemical precipitation method, electrochemical process, absorption method and membrane separation process etc. at present, also has some new technology as nanometer technology, photocatalytic method, New Type of Mesoporous material and gene treatment technology etc.Oyster shell whiting is as a kind of natural cleaning material of cheapness, be a kind of respond well adsorbent, the oyster shell whiting utilizing natural seashell to make becomes the wastewater treatment means of a kind of high-efficiency environment friendly in recent years to the technology processing heavy metal pollution in wastewater and is subject to common concern.But current oyster shell whiting limited sorption capacity, therefore makes it apply and is extremely restricted.
The Chinese patent of application publication number CN103585950A, Shen Qing Publication day 2014.02.19 discloses a kind of preparation method of natural shell adsorbent, comprises the steps: that (1) cleans organic matter and the inorganic pollution of shell surface with acid solution; (2) shell of cleaning gained is dried and calcined; (3) tentatively pulverize calcining the oven dry shell obtained; (4) carry out deep layer pulverizing to tentatively pulverizing the shell obtained, grind and sieve and obtain oyster shell whiting, again low temperature presintering is carried out to oyster shell whiting, its moisture is evaporated, abundant dehydration, (5) first TiO2 colloidal sol is prepared, again will through this TiO2 peptization of shell powder load that obtains of dewatering, the steps such as drying successively-rinse-dry-fuse, obtain the immobilized TiO of oyster shell whiting
2.The method carrys out load to improve the adsorption effect of oyster shell whiting by TiO2 colloidal sol, and TiO2 dissolved adhesiveness is large, and oyster shell whiting is difficult to be uniformly dispersed at TiO2 colloidal sol, thus makes TiO
2on oyster shell whiting, load is uneven, causes the absorption property heterogeneity of oyster shell whiting.
Summary of the invention
The object of this invention is to provide the preparation method in order to a kind of modification oyster shell whiting, the oyster shell whiting be processed into shell is primary raw material, and pass through carbon nano-tube modification, greatly improve the adsorption capacity of its heavy metal ion, improve oyster shell whiting utilization rate, exploitation natural adsorbent and effluent containing heavy metal ions improvement in provide an effective way.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for modification oyster shell whiting, comprises the following steps:
(1) oyster shell whiting is prepared
(1) being cleaned by shell in mass concentration is soak 30 ~ 40min in the hydrochloric acid solution of 0.1 ~ 0.3%, takes out and drains rear high-temperature calcination 1 ~ 2h, wash, dry, cross 120 ~ 200 mesh sieves, obtain oyster shell whiting after pulverizing.Shell raw material can be the shell of the various shellfishes such as nacre, scallop, mussel, oyster, razor clam, without particular/special requirement; By salt acid soak to remove the organic and inorganic impurity in surface; By high-temperature calcination to remove the organic matter of shell inside.
(2) oyster shell whiting is placed in the ethanolic solution that mass concentration is 30 ~ 40%, after sonic oscillation 10 ~ 15min, dries.Oyster shell whiting carries out sonic oscillation in ethanolic solution, thoroughly to remove the impurity on oyster shell whiting, thus is conducive to the attachment of CNT.
(2) modified carbon nano-tube is prepared
A CNT adds in chlorosulfonic acid by (), be heated to 80 ~ 100 DEG C of swelling 1 ~ 3h, cold filtration, filtrate deionized water is washed till pH in neutral, and at 1800 ~ 2000 DEG C, anneal in argon gas atmosphere 3 ~ 5h, namely obtains swelling CNT after being cooled to room temperature.Chlorosulfonic acid can intercalation, swelling carbon nano-tube bundle, CNT is separated from each other and the amorphous carbon material of its surperficial high reaction activity is come out, can be improved it dispersed, be conducive to again in subsequent step, these amorphous carbon materials fully being removed, thus be conducive to the absorption property improving CNT; CNT can be avoided to be oxidized under the high temperature conditions by argon shield; pass through high annealing; annealing can not only eliminate the metal of entrained with in CNT, metal oxide and other carbon impurity effectively; and make the defect in carbon nano tube structure obtain reparation to a certain extent, contribute to the absorption property improving CNT.
B swelling CNT is added mass fraction by () is in the lauryl sodium sulfate ethanolic solution of 1 ~ 2%, 30 ~ 60min is stirred under 80 ~ 90 DEG C of conditions, suction filtration, adds in the hydrogenperoxide steam generator of 30 ~ 40% after oven dry while stirring, in 60 ~ 80 DEG C of heated at constant temperature 8 ~ 10h, suction filtration, filtrate deionized water being washed till pH is transferred in the hydrochloric acid solution of 3 ~ 4mol/L after neutrality, suction filtration after sonic oscillation, filtrate deionized water is washed till pH in neutral, vacuum drying, obtains modified carbon nano-tube.The structure of CNT, character determines its excellent adsorption capacity, especially the absorption of heavy metal ion, it is utilized to carry out modification to oyster shell whiting, greatly can improve the adsorption capacity of oyster shell whiting, but CNT is very easily reunited, not easily disperse, therefore in the present invention by modification to improve the dispersiveness of CNT, the present invention carries out modification by lauryl sodium sulfate to swelling CNT, chain type alkyl in lauryl sodium sulfate is adsorbed on carbon nano tube surface by hydrophobic effect, sulfate radical in lauryl sodium sulfate adds the negative electricity of carbon nano tube surface, add the electrostatic repulsion forces between CNT, thus improve the dispersiveness of CNT, even carbon nanotube can be made to be scattered in water also can effectively avoid reuniting, utilize the strong oxidizing property of hydrogen peroxide to carry out removing impurities by oxidation to the amorphous carbon material in CNT simultaneously, the integrality of carbon nano tube structure is not only maintained while removal of impurities, also can improve the yield of CNT, and in conjunction with the further removal of impurities of method of non-oxide acid (hydrochloric acid) pickling, thus to obtain pure modified carbon nano-tube to ensure its adsorption effect.
(3) modification oyster shell whiting is prepared
Be add SDBS dispersant in the sodium hydroxide solution of 0.1 ~ 0.3% in mass concentration, modified carbon nano-tube is added under stirring, oyster shell whiting is added after being uniformly dispersed, continue stirring 30 ~ 60min, product is after suction filtration, sonic oscillation cleaning, use deionized water cleaning, drying, obtain modification oyster shell whiting.
As preferably, in step (2), the power 4 ~ 6W of sonic oscillation.
As preferably, in step (a), cooldown rate when CNT is cooled to room temperature is 3 ~ 5 DEG C/min.Cooldown rate is too fast, CNT easy fracture, thus affects absorption property.
As preferably, in step (b), the process conditions of sonic oscillation are: power 4 ~ 6W, duration of oscillation 1 ~ 2h.
As preferably, in step (three), the addition of SDBS dispersant is 0.3 ~ 0.5% of sodium hydroxide solution quality, and the addition of modified carbon nano-tube is 0.1 ~ 0.2% of sodium hydroxide solution quality, and the addition of oyster shell whiting is 1 ~ 2% of sodium hydroxide solution quality.
As preferably, in step (three), drying is freeze-day with constant temperature under 50 ~ 60 DEG C of conditions.
As preferably, in step (three), the process conditions of sonic oscillation cleaning are: power 4 ~ 6W, duration of oscillation 1 ~ 2h.
Therefore, the present invention has following beneficial effect: the oyster shell whiting that the present invention is processed into shell is for primary raw material, by modified carbon nano-tube, modification is carried out to oyster shell whiting, thus greatly to improve the adsorption capacity of oyster shell whiting heavy metal ion, improve oyster shell whiting utilization rate, exploitation natural adsorbent and effluent containing heavy metal ions improvement in provide an effective way.
Detailed description of the invention
Below by detailed description of the invention, the present invention will be further described.
Embodiment 1
(1) oyster shell whiting is prepared
(1) being cleaned by oyster shell in mass concentration is soak 30min in the hydrochloric acid solution of 0.1%, takes out and drains rear high-temperature calcination 1h, wash, dry, and crosses 120 mesh sieves, obtain oyster shell whiting after pulverizing.
(2) oyster shell whiting is placed in the ethanolic solution that mass concentration is 30%, after sonic oscillation 10min, dry, ultrasonic power is 4W.
(2) modified carbon nano-tube is prepared
A CNT adds in chlorosulfonic acid by (), be heated to 80 DEG C of swelling 1h, cold filtration, filtrate deionized water is washed till pH in neutral, at 1800 DEG C, anneal in argon gas atmosphere 3h, namely obtains swelling CNT after being cooled to room temperature with the cooldown rate of 3 DEG C/min.
B swelling CNT is added mass fraction by () is in the lauryl sodium sulfate ethanolic solution of 1%, 30min is stirred under 80 DEG C of conditions, suction filtration, adds in the hydrogenperoxide steam generator of 30% after oven dry while stirring, in 60 DEG C of heated at constant temperature 8h, suction filtration, filtrate deionized water being washed till pH is transferred in the hydrochloric acid solution of 3mol/L after neutrality, with suction filtration after the power ultrasonic of 4W vibration 1h, filtrate deionized water is washed till pH in neutral, vacuum drying, obtains modified carbon nano-tube.
(3) modification oyster shell whiting is prepared
Be add SDBS dispersant in the sodium hydroxide solution of 0.1% in mass concentration, modified carbon nano-tube is added under stirring, oyster shell whiting is added after being uniformly dispersed, continue to stir 30min, product is after suction filtration, sonic oscillation cleaning, clean by deionized water, dry, obtain modification oyster shell whiting, wherein the addition of SDBS dispersant is 0.3% of sodium hydroxide solution quality, the addition of modified carbon nano-tube is 0.1% of sodium hydroxide solution quality, and the addition of oyster shell whiting is 1% of sodium hydroxide solution quality.
Embodiment 2
(1) oyster shell whiting is prepared
(1) being cleaned by scallop shell in mass concentration is soak 40min in the hydrochloric acid solution of 0.3%, takes out and drains rear high-temperature calcination 2h, wash, dry, and crosses 200 mesh sieves, obtain oyster shell whiting after pulverizing.
(2) oyster shell whiting is placed in the ethanolic solution that mass concentration is 30 ~ 40%, after sonic oscillation 15min, dries, ultrasonic power 6W.
(2) modified carbon nano-tube is prepared
A CNT adds in chlorosulfonic acid by (), be heated to 100 DEG C of swelling 3h, cold filtration, filtrate deionized water is washed till pH in neutral, at 2000 DEG C, anneal in argon gas atmosphere 5h, namely obtains swelling CNT after being cooled to room temperature with the cooldown rate of 5 DEG C/min.
B swelling CNT is added mass fraction by () is in the lauryl sodium sulfate ethanolic solution of 2%, 60min is stirred under 90 DEG C of conditions, suction filtration, adds in the hydrogenperoxide steam generator of 40% after oven dry while stirring, in 80 DEG C of heated at constant temperature 10h, suction filtration, filtrate deionized water being washed till pH is transferred in the hydrochloric acid solution of 4mol/L after neutrality, with suction filtration after the power ultrasonic of 6W vibration 2h, filtrate deionized water is washed till pH in neutral, vacuum drying, obtains modified carbon nano-tube.
(3) modification oyster shell whiting is prepared
Be add SDBS dispersant in the sodium hydroxide solution of 0.3% in mass concentration, modified carbon nano-tube is added under stirring, oyster shell whiting is added after being uniformly dispersed, continue to stir 60min, product is after suction filtration, sonic oscillation cleaning, clean by deionized water, dry, obtain modification oyster shell whiting, wherein the addition of SDBS dispersant is 0.5% of sodium hydroxide solution quality, the addition of modified carbon nano-tube is 0.2% of sodium hydroxide solution quality, and the addition of oyster shell whiting is 2% of sodium hydroxide solution quality.
Embodiment 3
(1) oyster shell whiting is prepared
(1) being cleaned by mussel shell in mass concentration is soak 35min in the hydrochloric acid solution of 0.2%, takes out and drains rear high-temperature calcination 1.5h, wash, dry, and crosses 160 mesh sieves, obtain oyster shell whiting after pulverizing.
(2) oyster shell whiting is placed in the ethanolic solution that mass concentration is 35%, after sonic oscillation 12min, dries, ultrasonic power 5W.
(2) modified carbon nano-tube is prepared
A CNT adds in chlorosulfonic acid by (), be heated to 90 DEG C of swelling 2h, cold filtration, filtrate deionized water is washed till pH in neutral, at 1900 DEG C, anneal in argon gas atmosphere 4h, namely obtains swelling CNT after being cooled to room temperature with the cooldown rate of 4 DEG C/min.
B swelling CNT is added mass fraction by () is in the lauryl sodium sulfate ethanolic solution of 1.5%, 40min is stirred under 85 DEG C of conditions, suction filtration, adds in the hydrogenperoxide steam generator of 35% after oven dry while stirring, in 70 DEG C of heated at constant temperature 9h, suction filtration, filtrate deionized water being washed till pH is transferred in the hydrochloric acid solution of 3.5mol/L after neutrality, with suction filtration after the power ultrasonic of 5W vibration 1.5h, filtrate deionized water is washed till pH in neutral, vacuum drying, obtains modified carbon nano-tube.
(3) modification oyster shell whiting is prepared
Be add SDBS dispersant in the sodium hydroxide solution of 0.2% in mass concentration, modified carbon nano-tube is added under stirring, oyster shell whiting is added after being uniformly dispersed, continue to stir 40min, product is after suction filtration, sonic oscillation cleaning, clean by deionized water, dry, obtain modification oyster shell whiting, wherein the addition of SDBS dispersant is 0.4% of sodium hydroxide solution quality, the addition of modified carbon nano-tube is 0.15% of sodium hydroxide solution quality, and the addition of oyster shell whiting is 1.2% of sodium hydroxide solution quality.
Get the electroplating wastewater of four parts of 100ml from Ruian, Zhejiang cylinder factory, the pH of this electroplating wastewater is 3, and its primary chemical consists of: CN
-: 18mg/L, Cr
6+: 78mg/L, Cu
2+: 28mg/L, Zn
2+: 43mg/L, Ni
2+: 22mg/L, after regulating pH to 7 ~ 7.5, the modification oyster shell whiting in embodiment 1 ~ 3 and unmodified oyster shell powder (comparative example) is added respectively at 25 DEG C, addition is 20g/L, filter as liquid to be measured with quantitative filter paper after standing adsorption 24h, liquid atomic absorption spectrophotometer to be measured measures CN in solution
-, Cr
6+, Cu
2+, Zn
2+and Ni
2+concentration, calculate the absorption of oyster shell whiting heavy metal.Computing formula is: adsorption rate (%)=(C
0-C)/C
0× 100%, C in formula
0for the initial concentration (mg/L) of heavy metal ion; C is the residual concentration (mg/L) of heavy metal ion after absorption, and the adsorption rate obtained is as follows:
Embodiment 1:CN
-adsorption rate=99.84%, Cr
6+adsorption rate=99.87%, Cu
2+adsorption rate=98.49%, Zn
2+adsorption rate=99.92%, Ni
2+adsorption rate=99.68%.
Embodiment 2:CN
-adsorption rate=99.92%, Cr
6+adsorption rate=99.68%, Cu
2+adsorption rate=98.69%, Zn
2+adsorption rate=98.99%, Ni
2+adsorption rate=99.97%.
Embodiment 3:CN
-adsorption rate=99.82%, Cr
6+adsorption rate=99.52%, Cu
2+adsorption rate=98.69%, Zn
2+adsorption rate=99.15%, Ni
2+adsorption rate=99.88%.
Comparative example: CN
-adsorption rate=73.62%, Cr
6+adsorption rate=68.38%, Cu
2+adsorption rate=73.31%, Zn
2+adsorption rate=79.75%, Ni
2+adsorption rate=77.86%.
From above-mentioned data, the modification oyster shell whiting obtained by the present invention, to the oyster shell whiting highly significant of the treatment effect of heavy metal ion-containing waste water compared with non-modified, illustrates that the adsorption capacity of the modification oyster shell whiting heavy metal ion obtained by the present invention is improved greatly.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (7)
1. a preparation method for modification oyster shell whiting, is characterized in that, comprises the following steps:
(1) oyster shell whiting is prepared
(1) being cleaned by shell in mass concentration is soak 30 ~ 40min in the hydrochloric acid solution of 0.1 ~ 0.3%, takes out and drains rear high-temperature calcination 1 ~ 2h, wash, dry, cross 120 ~ 200 mesh sieves, obtain oyster shell whiting after pulverizing;
(2) oyster shell whiting is placed in the ethanolic solution that mass concentration is 30 ~ 40%, after sonic oscillation 10 ~ 15min, dries;
(2) modified carbon nano-tube is prepared
A CNT adds in chlorosulfonic acid by (), be heated to 80 ~ 100 DEG C of swelling 1 ~ 3h, cold filtration, filtrate deionized water is washed till pH in neutral, and at 1800 ~ 2000 DEG C, anneal in argon gas atmosphere 3 ~ 5h, namely obtains swelling CNT after being cooled to room temperature;
B swelling CNT is added mass fraction by () is in the lauryl sodium sulfate ethanolic solution of 1 ~ 2%, 30 ~ 60min is stirred under 80 ~ 90 DEG C of conditions, suction filtration, adds in the hydrogenperoxide steam generator of 30 ~ 40% after oven dry while stirring, in 60 ~ 80 DEG C of heated at constant temperature 8 ~ 10h, suction filtration, filtrate deionized water being washed till pH is transferred in the hydrochloric acid solution of 3 ~ 4mol/L after neutrality, suction filtration after sonic oscillation, filtrate deionized water is washed till pH in neutral, vacuum drying, obtains modified carbon nano-tube;
(3) modification oyster shell whiting is prepared
Be add SDBS dispersant in the sodium hydroxide solution of 0.1 ~ 0.3% in mass concentration, modified carbon nano-tube is added under stirring, oyster shell whiting is added after being uniformly dispersed, continue stirring 30 ~ 60min, product is after suction filtration, sonic oscillation cleaning, use deionized water cleaning, drying, obtain modification oyster shell whiting.
2. the preparation method of a kind of modification oyster shell whiting according to claim 1, is characterized in that, in step (2), and the power 4 ~ 6W of sonic oscillation.
3. the preparation method of a kind of modification oyster shell whiting according to claim 1, is characterized in that, in step (a), cooldown rate when CNT is cooled to room temperature is 3 ~ 5 DEG C/min.
4. the preparation method of a kind of modification oyster shell whiting according to claim 1, is characterized in that, in step (b), the process conditions of sonic oscillation are: power 4 ~ 6W, duration of oscillation 1 ~ 2h.
5. the preparation method of a kind of modification oyster shell whiting according to claim 1, it is characterized in that, in step (three), the addition of SDBS dispersant is 0.3 ~ 0.5% of sodium hydroxide solution quality, the addition of modified carbon nano-tube is 0.1 ~ 0.2% of sodium hydroxide solution quality, and the addition of oyster shell whiting is 1 ~ 2% of sodium hydroxide solution quality.
6. the preparation method of a kind of modification oyster shell whiting according to claim 1, is characterized in that, in step (three), drying is freeze-day with constant temperature under 50 ~ 60 DEG C of conditions.
7. the preparation method of a kind of modification oyster shell whiting according to claim 1, is characterized in that, in step (three), the process conditions of sonic oscillation cleaning are: power 4 ~ 6W, duration of oscillation 1 ~ 2h.
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| CN107892339B (en) * | 2017-11-23 | 2021-03-16 | 浙江海洋大学 | Preparation and application of aquatic product sewage treatment agent |
| CN107892339A (en) * | 2017-11-23 | 2018-04-10 | 浙江海洋大学 | A kind of aquatic products sewage-treating agent prepares and its application |
| CN107970876A (en) * | 2017-12-15 | 2018-05-01 | 浙江海洋大学 | A kind of preparation method that oyster shell whiting is modified with stearic acid |
| CN108163922A (en) * | 2017-12-29 | 2018-06-15 | 兰溪市哥特生物技术有限公司 | The preparation method of grass carp cultivation water modifying agent |
| CN108906872A (en) * | 2018-06-05 | 2018-11-30 | 杭州电子科技大学 | The method for administering waste water and heavy metal pollution of soil with calcining oyster shell powder |
| CN109054515A (en) * | 2018-08-01 | 2018-12-21 | 淮北庆丰涂料有限公司 | A kind of diatom ooze |
| CN108997785A (en) * | 2018-08-03 | 2018-12-14 | 李远奖 | A kind of preparation method of the nano modification conch meal with durable antibiotic |
| CN109129808A (en) * | 2018-10-17 | 2019-01-04 | 合肥隆扬环保科技有限公司 | A kind of preparation method of novel high-strength environment-friendly sheet |
| CN110975837A (en) * | 2019-12-23 | 2020-04-10 | 重庆大学 | Modified oyster shell, preparation method and application thereof |
| CN112591843A (en) * | 2020-12-26 | 2021-04-02 | 昆明理工大学 | Method for treating heavy metal-containing acidic wastewater by using waste |
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