CN103657593B - A kind of method of sunflower seed shell biomass carbon adsorbent, preparation method and removal water Methylene Blue - Google Patents
A kind of method of sunflower seed shell biomass carbon adsorbent, preparation method and removal water Methylene Blue Download PDFInfo
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- CN103657593B CN103657593B CN201310686422.4A CN201310686422A CN103657593B CN 103657593 B CN103657593 B CN 103657593B CN 201310686422 A CN201310686422 A CN 201310686422A CN 103657593 B CN103657593 B CN 103657593B
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Abstract
A kind of method of sunflower seed shell biomass carbon adsorbent, preparation method and removal water Methylene Blue, belong to technical field of waste water processing, water cleaning sunflower seed shell, dry, broken, be sized to 300 ~ 600 μm, then by sunflower seed shell particle and liquor zinci chloridi hybrid infusion, microwave treatment, gained sunflower seed shell biomass carbon, through pickling, washing, drying, namely obtains sunflower seed shell biomass carbon adsorbent.Gained adsorbent is for removing the method for methylene blue in waste, and the inventive method is simple to operate, and cost is low, high-efficiency environment friendly.
Description
Technical field
The invention belongs to technical field of waste water processing, relate to a kind of method utilizing adsorbent to remove methylene blue in waste, particularly relate to a kind of method utilizing sunflower seed shell biomass carbon adsorbent to remove methylene blue in waste.
Background technology
Methylene blue is a kind of heteroaromatic compound, belong to phenothiazines basic-dyeable fibre, be usually used in fiber crops, silk fabric, the dyeing of paper and the painted of bamboo and wood, can be used for manufacturing the aspects such as the dyeing of ink and biological, bacterial organisms, also can be used as chemical indicator and medicine.The a large amount of methylene blue of acute absorption can cause heart rate to increase, vomiting, shock and quadriplegia etc.In addition, the methylene blue of high dose also can cause the symptom of Heng Shi corpusculum anaemia or the change of other red cell morphologies, reduces red blood cell life span.
Biomass carbon, refers to a kind of living beings generated by cracking or imperfect combustion by the living beings being rich in carbon.Biomass carbon has larger specific area, and surface is containing more oxygen-content active functional group, may be used for the organic pollution in absorption effluent or soil and heavy metal, simultaneously with low cost because of it, be considered to a kind of sorbing material having broad prospect of application.Prepare with the carbon containing such as agriculture and forestry organic waste material, trade waste debirs the environmental pollution that biomass carbon not only can reduce solid waste, effectively can also realize the resource of these debirs.
Sunflower seeds is one of large oil crops in the world five.China is the big producing country of sunflower seeds, and 2011 annual productions are 231.3 ten thousand tons.Current sunflower seeds the most widely purposes sells as a kind of parched medicinal material, is also the most traditional a kind of purposes.Along with the progress of science and technology and the development of food industry, people continually develop the new edible and economic worth of sunflower seeds, and such as utilize polly seed nucleole to extract oil and make the products such as health products beverage, yogurt, sunflower seeds grouts can be used as feed etc.But all the time fewer to utilizing of sunflower seed shell, except doing fuel, direct discarded object of being used as is thrown away mostly.Sunflower seeds shell-containing rate is generally 22 ~ 40%, and for 2011, the annual production of sunflower seed shell was 50.9 ~ 92.5 ten thousand tons.If utilize it to prepare adsorbent, not only can turn waste into wealth, and the pollution that sunflower seed shell causes can be alleviated, achieve resource and the economic worth of sunflower seed shell simultaneously.Utilize the methylene blue in sunflower seed shell charcoal sorbent treatment waste water, effectively can remove the methylene blue in waste water, also reach the effect of the treatment of wastes with processes of wastes against one another.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of adsorbent of removal methylene blue in waste of efficient, low cost.
Second technical problem to be solved by this invention is to provide a kind of method of removal methylene blue in waste of efficient, low cost.
A kind of sunflower seed shell biomass carbon adsorbent, for the sunflower seed shell of microwave treatment is as adsorbent.
The preparation method of above-mentioned sunflower seed shell biomass carbon adsorbent comprises the following steps:
Sunflower seed shell is cleaned with running water, dry, broken, be sized to 300 ~ 600 μm, again by sunflower seed shell particle and liquor zinci chloridi hybrid infusion, microwave treatment, with hydrochloric acid solution pickling gained sunflower seed shell biomass carbon, then cleans to pH in neutral with distilled water, drying, namely obtains sunflower seed shell biomass carbon adsorbent.
The concentration of above-mentioned liquor zinci chloridi preferably 55% ~ 75%, preferred sunflower seed shell particle (g) of impregnating ratio of sunflower seed shell particle and liquor zinci chloridi: liquor zinci chloridi (g) is 1:5 ~ 1:7, microwave power is 480 ~ 640W preferably, microwave treatment time is 10 ~ 15min preferably, the concentration of hydrochloric acid solution preferably 10%.
Sunflower seed shell biomass carbon adsorbent described above, for removing the method for methylene blue in waste, comprises the following steps:
In containing the solution of methylene blue, add sunflower seed shell biomass carbon adsorbent and sodium chloride, adsorb 2 ~ 24h at 20 ~ 60 DEG C after, isolated by filtration, filtrate is adjusted to neutral rear discharge.
Concentration 100 ~ the 900mg/L, the pH value of solution that preferably contain the Methylene Blue in Solution of methylene blue are 2 ~ 12, and sunflower seed shell biomass carbon adsorbent amount is 2 ~ 5g/L, and the mass percent concentration of sodium chloride is no more than 30%.
Compared with prior art, the invention has the advantages that: compared with the methods such as ion-exchange, UF membrane, precipitation, the method for removal methylene blue in waste of the present invention is simple to operate, and cost is low, high-efficiency environment friendly.Sunflower seed shell biomass carbon adsorbent amount of the present invention is large, methylene blue adsorption value is 384.64mg/g, far exceed Wooden activated carbon for water purification national standard (135mg/g, National Standard of the People's Republic of China GB13803.2-1999), open the new way of sunflower seed shell recycling simultaneously.
Accompanying drawing explanation
Fig. 1 is the impact of pH on methylene blue removal effect.
Fig. 2 is the impact of methylene blue initial concentration on methylene blue removal effect.
Fig. 3 is the impact of sodium chloride concentration on methylene blue removal effect.
Fig. 4 is Langmuir adsorption isotherm.
Fig. 5 is the infrared spectrogram of sunflower seed shell biomass carbon adsorbent of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but the present invention is not restricted to embodiment.
Embodiment 1
Get the sunflower seed shell of certain mass, tap water for several times, dry, broken, be sized to 300 ~ 600 μm, by sunflower seed shell particle and liquor zinci chloridi according to sunflower seed shell granular mass (g): the ratio hybrid infusion that liquor zinci chloridi quality (g) is 1:7 is in conical flask, and wherein the concentration of liquor zinci chloridi is 55%.After 480W microwave treatment 15min, be the hydrochloric acid solution pickling gained sunflower seed shell biomass carbon of 10% by concentration, then clean to pH in neutral with distilled water, dry, namely obtain sunflower seed shell biomass carbon adsorbent.
Get adsorbent prepared by 0.1g the present embodiment and 5g sodium chloride to add solution ph and be respectively 2,4,6,7,8,10,12, in the methylene blue solution of 50mL, 100mg/L, after the 2h that vibrates in water bath with thermostatic control shaking table at 20 DEG C, isolated by filtration, filtrate is adjusted to neutral rear discharge.
Different initial pH on the impact of methylene blue removal effect as shown in Figure 1, can find out that pH is very little on the impact of methylene blue adsorption value, illustrate that the method for removal methylene blue of the present invention does not limit by pH substantially.
Embodiment 2
Get the sunflower seed shell of certain mass, tap water for several times, dry, broken, be sized to 300 ~ 600 μm, by sunflower seed shell particle and liquor zinci chloridi according to sunflower seed shell granular mass (g): the ratio hybrid infusion that liquor zinci chloridi quality (g) is 1:6.5 is in conical flask, and wherein the concentration of liquor zinci chloridi is 60%.After 520W microwave treatment 14min, be the hydrochloric acid solution pickling gained sunflower seed shell biomass carbon of 10% by concentration, then clean to pH in neutral with distilled water, dry, namely obtain sunflower seed shell biomass carbon adsorbent.
Get adsorbent prepared by 0.15g the present embodiment and 2.5g sodium chloride add respectively containing 100,300,500,700, in the 50mL solution of 900mg/L methylene blue, after the 24h that vibrates in water bath with thermostatic control shaking table at 20 DEG C, isolated by filtration, filtrate be adjusted to neutral after discharge.
Methylene blue initial concentration on the impact of methylene blue removal effect as shown in Figure 2.Under the driving of concentration gradient, along with methylene blue initial concentration is increased to 700mg/L by 100mg/L, methylene blue adsorption value rises to 343.27mg/g by 51.21mg/g, and clearance only drops to 97.60% by 99.82%.When methylene blue initial concentration is 900mg/L, methylene blue adsorption value is 392.80mg/g, and clearance is 87.45%.This shows that the method for removal methylene blue of the present invention is applicable to the wastewater treatment containing 100 ~ 700mg/L methylene blue.
Embodiment 3
Get the sunflower seed shell of certain mass, tap water for several times, dry, broken, be sized to 300 ~ 600 μm, by sunflower seed shell particle and liquor zinci chloridi according to sunflower seed shell granular mass (g): the ratio hybrid infusion that liquor zinci chloridi quality (g) is 1:6 is in conical flask, and wherein the concentration of liquor zinci chloridi is 65%.After 560W microwave treatment 13min, be the hydrochloric acid solution pickling gained sunflower seed shell biomass carbon of 10% by concentration, then clean to pH in neutral with distilled water, dry, namely obtain sunflower seed shell biomass carbon adsorbent.
Get adsorbent 0.20g prepared by the present embodiment to add sodium chloride and make its mass percent concentration be respectively 0%, 2%, 5%, 10%, 15%, 30%, in the methylene blue solution of 50mL, 100mg/L, vibrate in water bath with thermostatic control shaking table at 20 DEG C after 2h, isolated by filtration, filtrate is adjusted to neutral rear discharge.
Sodium chloride concentration on the impact of methylene blue removal effect as shown in Figure 3.When sodium chloride concentration is higher, (15% and 30%) rate of adsorption is very fast, but different sodium chloride concentration is not remarkable on the impact of adsorbance, sunflower seed shell biomass carbon adsorbent (0% ~ 30%) can realize the Adsorption to methylene blue within the scope of wider sodium chloride concentration.
Embodiment 4
Get the sunflower seed shell of certain mass, tap water for several times, dry, broken, be sized to 300 ~ 600 μm, by sunflower seed shell particle and liquor zinci chloridi according to sunflower seed shell granular mass (g): the ratio hybrid infusion that liquor zinci chloridi quality (g) is 1:5.5 is in conical flask, and wherein the concentration of liquor zinci chloridi is 70%.After 600W microwave treatment 12min, be the hydrochloric acid solution pickling gained sunflower seed shell biomass carbon of 10% by concentration, then clean to pH in neutral with distilled water, dry, namely obtain sunflower seed shell biomass carbon adsorbent.
Get adsorbent prepared by 0.25g the present embodiment and 2.5g sodium chloride joins 50mL respectively containing 100,300,500,700, in the solution of 900mg/L methylene blue, in 20 DEG C, 40 DEG C, vibrate in water bath with thermostatic control shaking table at 60 DEG C after 21h, isolated by filtration, filtrate is adjusted to neutral rear discharge.
Absorption result Langmuir adsorption isotherm matching, as shown in Figure 4, fitting result is as shown in table 1 for the adsorption isotherm under different temperatures.
As can be seen from Fig. 4 and table 1, Langmuir model is fine to the fitting effect of the isothermal adsorption test data of methylene blue to sunflower seed shell biomass carbon adsorbent, and therefore Langmuir model can describe the isothermal adsorption test data of sunflower seed shell biomass carbon adsorbent to methylene blue well.As can be seen from Table 1, Q0 and b all declines along with the rising of temperature, this shows that the surface-active of sunflower seed shell biomass carbon adsorbent declines along with the rising of temperature, have higher compatibility under cryogenic with methylene blue molecule, namely sunflower shell biomass carbon adsorbent is better to the adsorption effect of methylene blue under cryogenic.Show technological process of the present invention to operating condition and equipment requirement low, be the wastewater containing methylene blue processing method of a kind of economy, economize energy, be suitable for propagation and employment.
When 20 DEG C, the maximum mono layer adsorption amount Q of the sunflower seed shell biomass carbon adsorbent methylene blue calculated with Langmuir thermoisopleth
0384.62mg/g, far exceed Wooden activated carbon for water purification national standard (135mg/g, National Standard of the People's Republic of China GB13803.2-1999), illustrate that modification sunflower seed shell of the present invention can as the adsorbent of a kind of high efficiency, low cost of process wastewater containing methylene blue.
Table 1Langmuir adsorption isotherm parameter
Embodiment 5
Get the sunflower seed shell of certain mass, tap water for several times, dry, broken, be sized to 300 ~ 600 μm, by sunflower seed shell particle and liquor zinci chloridi according to sunflower seed shell granular mass (g): the ratio hybrid infusion that liquor zinci chloridi quality (g) is 1:5 is in conical flask, and wherein the concentration of liquor zinci chloridi is 75%.After 640W microwave treatment 10min, be the hydrochloric acid solution pickling gained sunflower seed shell biomass carbon of 10% by concentration, then clean to pH in neutral with distilled water, dry, namely obtain sunflower seed shell biomass carbon adsorbent.
Infrared spectrum analysis is carried out to sunflower seed shell biomass carbon adsorbent prepared by the present embodiment.
Infrared spectrogram such as Fig. 5 of sunflower seed shell biomass carbon adsorbent prepared by the present embodiment shows.3429cm
-1the stretching vibration of O – H in the absworption peak representation hydroxy at place, 2924cm
-1absworption peak be CH in C – H and cellulose and hemicellulose in aliphatic compound
2the overlap of stretching vibration, 1694cm
-1the absworption peak at place is caused by the vibration of C=O in carbonyl, 1617cm
-1the absworption peak at place may be the stretching vibration of C=O, 1409cm
-1the absworption peak at place is the coefficient result of deformation vibration of O – H in the symmetrical stretching vibration of C=O in ester and alcohol, 1223cm
-1the absworption peak at place may be C – N(III type amido) stretching vibration causes, 1094cm
-1the absworption peak at place is the superposition of the stretching vibration of C – O – C in P – O – C and polysaccharose substance in phosphonyl group, and the absworption peak of its all band (in figure near finger print) is the vibration of phosphonyl group or sulphur group.The above results shows, sunflower seed shell biomass carbon adsorbent surface is rich in hydroxyl, carbonyl isoreactivity group.
Claims (5)
1. a sunflower seed shell biomass carbon adsorbent is for removing the method for methylene blue in waste, it is characterized in that, comprise the following steps: in containing the solution of methylene blue, add sunflower seed shell biomass carbon adsorbent and sodium chloride, adsorb 2 ~ 24h at 20 ~ 60 DEG C after, isolated by filtration, filtrate is adjusted to neutral rear discharge, be 2 ~ 12 containing the concentration 100 ~ 900mg/L of the Methylene Blue in Solution of methylene blue, pH value of solution, sunflower seed shell biomass carbon adsorbent amount is 2 ~ 5g/L, and the mass percent concentration of sodium chloride is no more than 30%;
The wherein preparation method of sunflower seed shell biomass carbon adsorbent, comprise the following steps: clean sunflower seed shell with running water, drying, broken, be sized to 300 ~ 600 μm, then by sunflower seed shell particle and liquor zinci chloridi hybrid infusion, microwave treatment, microwave power is 480 ~ 640W, with hydrochloric acid solution pickling gained sunflower seed shell biomass carbon, then cleans to pH in neutral with distilled water, drying, namely obtains sunflower seed shell biomass carbon adsorbent.
2. according to the method for claim 1, it is characterized in that, the mass percent concentration of liquor zinci chloridi is 55% ~ 75%.
3. according to the method for claim 1, it is characterized in that, the dipping of sunflower seed shell particle and liquor zinci chloridi is sunflower seed shell particle according to mass ratio: liquor zinci chloridi is 1:5 ~ 1:7.
4. according to the method for claim 1, it is characterized in that, microwave treatment time is 10 ~ 15min.
5. according to the method for claim 1, it is characterized in that, hydrochloric acid solution mass percent concentration is 10%.
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| CN105080500A (en) * | 2015-05-18 | 2015-11-25 | 江苏大学 | Natural dye wastewater adsorbent and preparation and application method thereof |
| CN107930573A (en) * | 2017-11-29 | 2018-04-20 | 华东交通大学 | One kind removes methylene blue adsorption number agent |
| CN109482155A (en) * | 2018-12-13 | 2019-03-19 | 重庆工商大学 | Preparation method of modified sunflower seed shell biological adsorption agent and products thereof and application |
| CN112263993B (en) * | 2020-10-19 | 2023-08-25 | 大连海事大学 | Boron-phosphorus co-doped activated carbon for adsorption of aromatic ring-containing compound in water and preparation method thereof |
| CN112457853B (en) * | 2020-11-25 | 2022-01-07 | 河南省科学院高新技术研究中心 | Zinc-rich biochar, preparation method thereof and application of zinc-rich biochar in passivation and remediation of heavy metal contaminated soil |
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