CN104492386A - Preparation method for oxalic-acid-modified pummelo pericarp biological adsorbent - Google Patents
Preparation method for oxalic-acid-modified pummelo pericarp biological adsorbent Download PDFInfo
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- CN104492386A CN104492386A CN201410601867.2A CN201410601867A CN104492386A CN 104492386 A CN104492386 A CN 104492386A CN 201410601867 A CN201410601867 A CN 201410601867A CN 104492386 A CN104492386 A CN 104492386A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
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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
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Abstract
A related preparation method for an oxalic-acid-modified pummelo pericarp biological adsorbent comprises the following steps: step (1) cleaning crude pummelo pericarp (PP), baking, crushing and sieving; step (2), getting the crude pummelo pericarp (PP) prepared in the step (1), adding isopropanol, immersing with stirring, and performing pumping filtration; step (3) baking the pummelo pericarp subjected to pumping filtration in the step (2), so as to obtain a pummelo pericarp adsorbent (PP1); step (4), immersing the pummelo pericarp adsorbent (PP1) obtained in the step (3) with NaOH, neutralizing and performing pumping filtration, and baking to obtain a pummelo pericarp adsorbent (PP2); and step (5) adding 1% of oxalic acid into the pummelo pericarp adsorbent (PP2) obtained in the step (4), immersing with stirring, performing pumping filtration, and baking, so as to obtain the modified pummelo pericarp adsorbent (MPP). New application of pummelo pericarp is discovered by performing adsorption research on a heavy metal cadmium by using oxalic-acid-modified pummelo pericarp.
Description
Technical field
The present invention relates to a kind of preparation method of oxalic acid modification pomelo peel biological adsorption agent, belong to technical field of environmental material preparation.
Background technology
The water pollutions that in industrial wastewater, each heavy metal species causes just is receiving the concern in the world.Heavy metal ion is mainly discharged in natural environment by industrial wastewater, urban domestic wastewater and various mining wastewaters such as smelting, electrolysis and plating.Wherein, the pollution of cadmium metal particularly needs to pay attention to, and a considerable amount of cadmium enters environment by waste gas, waste water, waste residue, pollutes.Pollution sources are Pb-Zn deposits mainly, and non-ferrous metal metallurgy, plating and make the factory of raw material or catalyst of cadmium compound.Cadmium can not biodegradation and thermal degradation at nature, and enter human body by food chain, very harmful to the internal organ such as human kidney, lung, cadmium can damage renal tubule, makes people occur the symptoms such as glycosuria, albuminuria and acidaminuria, and the discharge rate of urine calcium and uric acid is increased.Renal insufficiency can affect again the activity of vitamine D3, makes the growth metabolism of bone interrupted, thus causes skeleton bulking, atrophy, distortion etc., can cause anaemia at people's body accumulation.Traditional heavy metal containing wastewater treatment technology mainly contains chemical precipitation, chemical oxidation and reduction, ion-exchange, membrane technology, electrochemical treatments, counter-infiltration and distillation etc., there is the problem of secondary pollution in these traditional methods, particularly as the heavy metal concentration in the aqueous solution lower (< 100mg/L), not only clearance is lower, and operating cost is higher.Therefore, find a kind of green sewage purification material of comparatively cheapness, high adsorption capacity, become focus and the difficult point of research at present.
In recent years, have much about the research of agricultural wastes reproducing adsorbent Adsorption of Heavy Metals.And the main component of pomelo peel is made up of materials such as cellulose, hemicellulose, lignin and pectin, because these composition surfaces are containing a large amount of active function groups, can be combined by modes such as ion-exchange, chelating and complexings with metal ion, thus for the purification of heavy metal ion in the aqueous solution, existing scholar it can be used as pollutant absorbent both at home and abroad, is mainly used in the absorption of Cr.But about utilizing oxalic acid, the pomelo peel modification after saponification process be have not been reported to prepare biological adsorption agent due to the cadmium ion in Adsorption industrial wastewater.For this reason, this test adopts pomelo peel to be adsorbent material, and using oxalic acid as modifier, prepared modification shaddock peel adsorbent, preparation is simple, only need soak it, dries, grind.Study its adsorption capacity to Cd (II), and its adsorption dynamics adsorption kinetics and thermodynamic characteristics are inquired into, be intended to verify oxalic acid modification pomelo peel to the adsorption capacity of Cd in water (II) and influence factor thereof, to providing a feasible way for the recycling of pomelo peel, and for adsorption method for purifying sewage adsorbent screening theoretical foundation is provided.
Summary of the invention
The present invention, using oxalic acid as modifier, has prepared modification pomelo peel biological adsorption agent.Prepared adsorbent is used for the Cd (II) in Adsorption industrial wastewater.
Technical scheme
1, by thick pomelo peel (PP) after running water and distilled water are cleaned in 70 DEG C of thermostatic drying chambers, dry 24h, pulverize, cross 100 mesh sieves, store for subsequent use;
2, the thick pomelo peel (PP) 50 grams getting in step 1 preparation is placed in beaker, add 1000mL, 30% isopropyl alcohol, soaking at room temperature stirs 24h, and suction filtration, is washed till colourless with distilled water;
3, after step 2 obtains pomelo peel suction filtration, this sample is placed in the thermostatic drying chamber of 70 DEG C, dries 24h, obtain shaddock peel adsorbent (PP1);
4, shaddock peel adsorbent (PP1) 30g step 3 obtained is placed in beaker, add 500mL, mass fraction be 1% NaOH soaking and stirring 24h, suction filtration, pH value weakly acidic pH is washed till with distilled water, after suction filtration, sample is placed in the thermostatic drying chamber of 70 DEG C, dries 24h, obtain shaddock peel adsorbent (PP2).
5, shaddock peel adsorbent (PP2) 20g step 4 obtained is placed in beaker, add 500mL, 1% oxalic acid, soaking and stirring 24h, suction filtration, then wash repeatedly with distillation, after suction filtration, sample is placed in the thermostatic drying chamber of 70 DEG C, dry 24h, obtain modification shaddock peel adsorbent (MPP).
As a total inventive concept, the present invention also provides the application of above-mentioned biological adsorption agent, as the biological adsorption agent that above-mentioned preparation technology prepares is for a method for Cd (II) Adsorption, first configures Cd (II) standard reserving solution (1g/L): by 3CdSO
48H
2o H
2sO
4(1: 1, V/V) dissolves secondary deionized water constant volume and obtains, and other standards solution series is formed by standard reserving solution stepwise dilution.In 100mL tool plug conical flask, add modification pomelo peel biological adsorption agent 0.05g and Cd (II) the solution 10mL of preparation, regulate pH value of solution to 5.0 with 1.0mol/LHCL and 1.0mol/LNaOH.Putting it in water-bath constant temperature oscillator vibrates after 1.5 ~ 2h with 150r/min under normal temperature condition filters, and measures Cd (II) equilibrium concentration in filtrate with atomic absorption spectrophotometer.Adsorption rate (E%) and adsorbance (q, mg/g) calculate according to following formula.
E％＝[(C
0-C
e)/C
0]×100％ (1)
q＝[(C
0-C
e)V]/W (2)
C
0and C (mg/L)
e(mg/L) be respectively concentration during initial concentration and the balance of Cd (II), V (L) and W (g) is respectively the dosage of liquor capacity and adsorbent.
Beneficial effect
1. the present invention uses agricultural wastes pomelo peel to manufacture biological adsorption agent heavy-metal ion removal pollutant, with low cost, and technique is simple, has very large value.
2. the present invention has carried out adsorbing research to pomelo peel modification heavy metal cadmium by oxalic acid, has found the new purposes of pomelo peel, has extended the applicable object of pomelo peel, added the use value of pomelo peel.
3. of the present inventionly reach the efficient removal of heavy metal cadmium by oxalic acid to pomelo peel modification, clearance is the highest can reach 97%, reaches extraordinary effect.
Accompanying drawing explanation
Infrared spectrum before and after oxalic acid modification pomelo peel biological adsorption agent absorption Cd (II) prepared by Fig. 1.From Fig. 1, the known prepared modification biological adsorbent surface of a curve contains abundant hydroxyl, carboxyl, carbonyl isoreactivity group.From Fig. 1, the known-OH of b curve, C-H ,-COOH-,-C=0 group are the main functional group participating in absorption, realize adsorbing by carrying out complexing or chelating with Cd (II).
The different pH value of Fig. 2 is on the impact of modification biological adsorbent Cd (II).As can be seen from Figure 2, the increase modification biological adsorbent adsorption rate to Cd (II) of pH along with pH value between 1.0-5.0 increases gradually, and when pH value is increased to 5.0, adsorption rate is maximum, pH value more than 5.0 along with the increase adsorption rate of pH value reduces.
Detailed description of the invention
(1), the preparation of oxalic acid modification pomelo peel biological adsorption agent
1, by thick pomelo peel (PP) after running water and distilled water are cleaned in 70 DEG C of thermostatic drying chambers, dry 24h, pulverize, cross 100 mesh sieves, store for subsequent use;
2, the thick pomelo peel (PP) 50 grams getting in step 1 preparation is placed in beaker, add 1000mL, 30% isopropyl alcohol, soaking at room temperature stirs 24h, and suction filtration, is washed till colourless with distilled water;
3, after step 2 obtains pomelo peel suction filtration, this sample is placed in the thermostatic drying chamber of 70 DEG C, dries 24h, obtain shaddock peel adsorbent (PP1);
4, shaddock peel adsorbent (PP1) 30g step 3 obtained is placed in beaker, add 500mL, mass fraction be 1% NaOH soaking and stirring 24h, suction filtration, pH value weakly acidic pH is washed till with distilled water, after suction filtration, sample is placed in the thermostatic drying chamber of 70 DEG C, dries 24h, obtain shaddock peel adsorbent (PP2).
5, shaddock peel adsorbent (PP2) 20g step 4 obtained is placed in beaker, add 500mL, 1% oxalic acid, soaking and stirring 24h, suction filtration, then wash repeatedly with distillation, after suction filtration, sample is placed in the thermostatic drying chamber of 70 DEG C, dry 24h, obtain modification shaddock peel adsorbent (MPP).
(2) to the absorption property evaluation of cadmium (II)
In the present invention, in specific embodiments, absorption property evaluation is carried out by the following method: first configure Cd (II) standard reserving solution (1g/L), modification pomelo peel biological adsorption agent 0.05g and Cd (II) solution 10mL is added in 100mL tool plug conical flask, pH value of solution to 5.0 is regulated with 1.0mol/LHCL and 1.0mol/LNaOH, putting it in water-bath constant temperature oscillator vibrates after 1.5 ~ 2h with 150r/min under normal temperature condition filters, and measures Cd (II) equilibrium concentration in filtrate with atomic absorption spectrophotometer.Each experiment all adopts two parallel laboratory test, and data are averaged.Adsorption rate (E%) and adsorbance (q, mg/g) calculate according to following formula.
E％＝[(C
0-C
e)/C
0]×100％ (1)
q＝[(C
0-C
e)V]/W (2)
C
0and C (mg/L)
e(mg/L) be respectively concentration during initial concentration and the balance of Cd (II), V (L) and W (g) is respectively the dosage of liquor capacity and adsorbent.
Below in conjunction with concrete embodiment, the present invention will be further described.
Test example 1: adding concentration respectively in a series of 100mL tool plug conical flask is: 5,10,30,50,100,150,200,250,300,350, Cd (II) solution of 400mg/L, regulate pH=5.0, at 25 DEG C, 35 DEG C and 40 DEG C, empirically method carries out adsorption experiment respectively, calculates its adsorption capacity q (mg/g) according to formula 2.Along with the increase of equilibrium concentration, MPP is to the adsorption capacity q of Cd (II)
efirst increase sharply, increase slowly subsequently, finally reach balance.Maximum monolayer capacity under pH=5.0,25 DEG C of conditions is 33.12mg/g.
Test example 2: add concentration and be respectively in a series of 100mL tool plug conical flask: the Cd (II) of 50mg/L, 100mg/L, 150mg/L, regulate pH=5.0, add 0.25g biological adsorption agent MPP under 25 DEG C of room temperatures respectively and carry out adsorption experiment, vibrate 10,20,30,45,60,120 and 300min respectively, supernatant liquor is got centrifugal after leaving standstill 2h, by the equilibrium concentration of FAAS spectrographic determination Cd (II), calculate its adsorption capacity Q (mg/g).Result shows, biological adsorption agent MPP has good adsorption dynamics adsorption kinetics performance to Cd (II), substantially reaches adsorption equilibrium in 1 hour.
Test example 3: add Cd (II) solution that concentration is 100mg/L in a series of 100mL tool plug conical flask, regulate pH=5.0,0.05g is added respectively under 25 DEG C of conditions, 0.10g, 0.15g, 0.20g, 0.25g, 0.30g, 0.40g biological adsorption agent MPP carries out adsorption experiment, when the dosage of MPP is less than 0.25g, along with the increase of dosage, Cd (II) clearance increases sharply, because along with the increase of adsorbent dosage, the total specific area of adsorbent and functional group also increase thereupon, therefore can improve Cd (II) clearance.After the dosage of adsorbent MPP reaches 0.25g, clearance reaches more than 95%, is up to 97%, substantially reaches adsorption equilibrium; But unit adsorbance declines along with increasing of MPP consumption.
Above-described embodiment is further described foregoing of the present invention, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is only limitted to above-described embodiment.All technology realized based on foregoing all belong to scope of the present invention.
Claims (8)
1. a preparation technology for oxalic acid modification pomelo peel biological adsorption agent, is characterized in that: it comprises following steps,
(1) thick pomelo peel (PP) is cleaned, dries, pulverizes, sieved;
(2): the thick pomelo peel (PP) getting preparation in step (1), adds isopropyl alcohol, soaking and stirring, suction filtration;
(3): step (2) obtains pomelo peel after suction filtration, is dried by this sample, obtains shaddock peel adsorbent (PP1);
(4): shaddock peel adsorbent (PP1) NaOH step (3) obtained soaks, in and suction filtration after, dry to obtain shaddock peel adsorbent (PP2);
(5): the shaddock peel adsorbent (PP2) step (4) obtained adds the oxalic acid of 1%, soaking and stirring, suction filtration, dry, obtain modification shaddock peel adsorbent (MPP).
2. preparation technology according to claim 1, is characterized in that step (1) is as follows: by thick pomelo peel (PP) after running water and distilled water are cleaned in 70 DEG C of thermostatic drying chambers, dry 24h, pulverize, cross 100 mesh sieves, store for subsequent use.
3. preparation technology according to claim 1, it is characterized in that step (2) is as follows: the thick pomelo peel (PP) 50 grams getting preparation in step (1) is placed in beaker, add 1000mL, 30% isopropyl alcohol, soaking at room temperature stirs 24h, suction filtration, is washed till colourless with distilled water.
4. preparation technology according to claim 1, it is characterized in that step (3) is as follows: after step (2) obtains pomelo peel suction filtration, this sample is placed in the thermostatic drying chamber of 70 DEG C 2, dries 24h, obtain shaddock peel adsorbent (PP1).
5. preparation technology according to claim 1, it is characterized in that step (4) is as follows: shaddock peel adsorbent (PP1) 30g step (3) obtained is placed in beaker, add 500mL, mass fraction be 1% NaOH soaking and stirring 24h, suction filtration, be washed till pH value weakly acidic pH with distilled water, after suction filtration, sample be placed in the thermostatic drying chamber of 70 DEG C, dry 24h, obtain shaddock peel adsorbent (PP2).
6. preparation technology according to claim 1, it is characterized in that step (5) is as follows: shaddock peel adsorbent (PP2) 20g step (4) obtained is placed in beaker, add 500mL, 1% oxalic acid, soaking and stirring 24h, suction filtration, then washes repeatedly with distillation, after suction filtration, sample is placed in the thermostatic drying chamber of 70 DEG C, dries 24h, obtain modification shaddock peel adsorbent (MPP).
7. the biological adsorption agent (MPP) for preparing of the oxalic acid modification pomelo peel biological adsorption agent preparation technology according to any one of claim 1-6 is for the purposes of the Adsorption of Cd (II).
8. according to claim 7 described purposes, it is characterized in that step is as follows:
Step 1, absorption: first configure Cd (II) standard reserving solution (1g/L): by 3CdSO
4gH
2o H
2sO
4(1: 1, V/V) dissolves secondary deionized water constant volume and obtains, and other standards solution series is formed by standard reserving solution stepwise dilution.In 100mL tool plug conical flask, add modification pomelo peel biological adsorption agent 0.05g and Cd (II) the solution 10mL of preparation, regulate pH value of solution to 5.0 with 1.0mol/LHCL and 1.0mol/LNaOH.Putting it in water-bath constant temperature oscillator vibrates after 1.5 ~ 2h with 150r/min under normal temperature condition filters, and measures Cd (II) equilibrium concentration in filtrate with atomic absorption spectrophotometer.Adsorption rate (E%) and adsorbance (q, mg/g) calculate according to following formula,
E％＝[(C0-C
e)/C
0]×100％ (1)
q＝[(C
0-C
e)V]/W (2)
C
0and C (mg/L)
e(mg/L) be respectively concentration during initial concentration and the balance of Cd (II), V (L) and W (g) is respectively the dosage of liquor capacity and adsorbent;
Step 2, desorb: precipitation after step 1 being filtered to be sent in 50mL colorimetric cylinder and added distilled water, adds 10mL1molL subsequently
-1hCl, be settled to the volume identical with the liquid before the precipitation in step 1, Cd (II) concentration in filtrate is measured after 25 DEG C-30 DEG C vibration 2.5-3h. filter, desorption efficiency is determined by the amount of the Cd (II) separating sucking-off in strippant, calculate biological adsorption agent to the desorption efficiency D of Cd (II)
H
de(mg/L) be Cd (II) concentration that in solution, desorb is got off, H
ad(mg/L) be Cd (II) concentration adsorbed on biological adsorption agent.
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Cited By (13)
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| CN105749873A (en) * | 2016-03-28 | 2016-07-13 | 柳州联海科技有限公司 | Adsorbent capable of efficiently recovering carbon monoxide and production method of adsorbent |
| CN106076301A (en) * | 2016-06-30 | 2016-11-09 | 信阳师范学院华锐学院 | The preparation method of succinic anhydride modified pomelo peel oil absorption material |
| CN106423076A (en) * | 2016-08-30 | 2017-02-22 | 运城学院 | Method for preparing PM2.5 (particulate matter 2.5) and TVOC (total volatile organic compound) purification biological absorbent from plant waste materials |
| CN106582557A (en) * | 2016-12-16 | 2017-04-26 | 常州市好利莱光电科技有限公司 | Preparation method for grapefruit peel-based low-concentration chromium-containing wastewater adsorbent |
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| CN107125653A (en) * | 2017-05-10 | 2017-09-05 | 福建农林大学 | The preparation method of pomelo peel Epigallo-catechin gallate (EGCG) compound |
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| CN104961268A (en) * | 2015-05-26 | 2015-10-07 | 北京科技大学 | Method for removing fluorine from underground water by using biomass coupled magnesium oxide |
| CN105749873A (en) * | 2016-03-28 | 2016-07-13 | 柳州联海科技有限公司 | Adsorbent capable of efficiently recovering carbon monoxide and production method of adsorbent |
| CN106076301B (en) * | 2016-06-30 | 2020-01-31 | 信阳学院 | Preparation method of succinic anhydride modified shaddock peel oil absorption material |
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| CN106423076A (en) * | 2016-08-30 | 2017-02-22 | 运城学院 | Method for preparing PM2.5 (particulate matter 2.5) and TVOC (total volatile organic compound) purification biological absorbent from plant waste materials |
| CN106582557A (en) * | 2016-12-16 | 2017-04-26 | 常州市好利莱光电科技有限公司 | Preparation method for grapefruit peel-based low-concentration chromium-containing wastewater adsorbent |
| CN106986522A (en) * | 2017-05-04 | 2017-07-28 | 浙江清天地环境工程有限公司 | A kind of flocculation dewatering agent and preparation method thereof |
| CN107175081A (en) * | 2017-05-04 | 2017-09-19 | 浙江清天地环境工程有限公司 | A kind of modification infusorial earth and preparation method thereof |
| CN107125653A (en) * | 2017-05-10 | 2017-09-05 | 福建农林大学 | The preparation method of pomelo peel Epigallo-catechin gallate (EGCG) compound |
| CN107349430A (en) * | 2017-07-04 | 2017-11-17 | 福建农林大学 | A kind of polysaccharide from Phyllanthus Emblica L EGCG compounds and preparation method thereof |
| CN107321311A (en) * | 2017-08-22 | 2017-11-07 | 河海大学 | A kind of phosphoric acid activation pomelo peel matrix activated carbon adsorbent and its preparation and application |
| CN107986498A (en) * | 2017-12-20 | 2018-05-04 | 北京科技大学 | The method of sulphion in a kind of precipitation-biological adsorption combination removing waste water |
| CN108741001A (en) * | 2018-04-28 | 2018-11-06 | 杨振华 | A kind of production method of sweet potato powder |
| CN111018038A (en) * | 2019-12-26 | 2020-04-17 | 浙江伊诺环保科技股份有限公司 | Heavy metal trapping agent and preparation process thereof |
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