CN110711560A - Preparation method of biomass adsorbent for printing and dyeing wastewater treatment - Google Patents
Preparation method of biomass adsorbent for printing and dyeing wastewater treatment Download PDFInfo
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- 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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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- 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
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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- 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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- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention relates to the field of adsorbent preparation, and discloses a preparation method of a biomass adsorbent for printing and dyeing wastewater treatment, which comprises the following steps: cleaning peanut shells, drying, crushing and sieving to obtain peanut shell powder; putting the peanut shell powder into a sodium hydroxide solution for swelling; adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting at 65-85 ℃ to obtain a first intermediate product; adding the first intermediate product into an ethylene diamine aqueous solution, and stirring and reacting at 80-90 ℃ to obtain a second intermediate product; and uniformly mixing the second intermediate product with a sodium alginate solution, adding epoxy chloropropane, reacting at 50-60 ℃, filtering and drying the product to obtain the biomass adsorbent. The biomass adsorbent prepared by modifying peanut shells as raw materials is low in cost, environment-friendly, high in viscosity, free of loosening phenomenon and high in adsorption efficiency on dyes and heavy metal ions.
Description
Technical Field
The invention relates to the field of preparation of adsorbents, and particularly relates to a preparation method of a biomass adsorbent for treating printing and dyeing wastewater.
Background
The printing and dyeing wastewater contains a large amount of toxic aromatic hydrocarbon derivatives with nitro, amino, sulfonic acid, chlorine-containing compounds and the like, and also contains acid, alkali, inorganic salt and heavy metal substances (metal mercury, chromium, zinc and the like), so that the printing and dyeing wastewater is a type of wastewater which is extremely harmful to the environment and difficult to treat. At present, the annual discharge amount of printing and dyeing wastewater in China is as high as 1.6 multiplied by 108t, only 22.5% was treated, and the yield was only 42%.
One of the remarkable characteristics of the printing and dyeing wastewater is that the wastewater has high chroma and poor water transparency, seriously influences the growth of aquatic organisms and microorganisms and is not beneficial to the self-purification of the water body. Therefore, decolorization is an important step in the treatment of printing and dyeing wastewater, the adsorption method is a conventional process for decolorizing printing and dyeing wastewater, and the most commonly used adsorbent mainly includes porous substances such as activated carbon and clay, for example, a method for adsorbing and decolorizing printing and dyeing wastewater by using attapulgite disclosed in chinese patent document, which is disclosed in publication No. CN101734745A, wherein the printing and dyeing wastewater is filtered by passing through the attapulgite or the attapulgite is added to the printing and dyeing wastewater, and the attapulgite adsorbs dye compounds in the printing and dyeing wastewater to achieve the decolorizing effect of the printing and dyeing wastewater.
However, when porous substances such as activated carbon, clay and the like are directly used as the adsorbent, the use cost is high, the regeneration is difficult, the phenomenon of loosening is easy to occur in the adsorption process, and the adsorption activity can not meet the requirement. In the face of such a critical and urgent environment, an effective, rapid, convenient and reproducible adsorbent is developed, which is one of effective solutions for solving the problem that dyes pollute water environment, improving the living standard of people and promoting the development of the environmental protection industry.
Disclosure of Invention
The invention provides a preparation method of a biomass adsorbent for printing and dyeing wastewater treatment, aiming at overcoming the problems that in the prior art, when porous substances such as activated carbon, clay and the like are used as an adsorbent in decolorization treatment in printing and dyeing wastewater treatment, the use cost is high, the regeneration is difficult, the adsorbent is easy to loose in the adsorption process, and the adsorption activity cannot meet the requirement.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a biomass adsorbent for printing and dyeing wastewater treatment comprises the following steps:
(1) cleaning peanut shells, drying, crushing and sieving to obtain peanut shell powder;
(2) putting the peanut shell powder into a sodium hydroxide solution for swelling;
(3) adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting at 65-85 ℃ to obtain a first intermediate product;
(4) adding the first intermediate product into an ethylene diamine aqueous solution, and stirring and reacting at 80-90 ℃ to obtain a second intermediate product;
(5) and uniformly mixing the second intermediate product with a sodium alginate solution, adding epoxy chloropropane, reacting at 50-60 ℃, filtering and drying the product to obtain the biomass adsorbent.
The cellulose rich in the peanut shells is a polyalcohol with active property, wherein the hydroxyl at the C2 position has higher acidity and is easy to generate etherification reaction, and the hydroxyl at the C6 position has stronger esterification capability. Therefore, the peanut shells can be subjected to esterification and etherification reactions under the physical and chemical actions to generate various types of cellulose ester and cellulose ether. The method comprises the steps of (1) and (2) placing the peanut shell powder obtained after cleaning, air drying, crushing and sieving in a sodium hydroxide solution for swelling, wherein a large amount of water molecules are arranged around the peanut shell powder due to strong hydration capacity of sodium ions and can be combined with cellulose macromolecules in the peanut shell powder under an alkaline condition, a large amount of water is substituted into cellulose to cause severe swelling of the cellulose, and meanwhile, hydroxyl groups on the cellulose react to generate a sodium alkoxide compound to generate alkaline cellulose with high reaction activity.
And (3) reacting the swelled peanut shell powder with acetic anhydride by using N, N-dimethylformamide as a solvent to obtain a first intermediate product, namely the peanut shell powder with the surface modified by acetic anhydride grafting, wherein a large amount of carboxyl is introduced after the acetic anhydride is grafted on the surface of the peanut shell powder. In the step (4), the first intermediate product reacts with ethylenediamine, amino groups can be introduced on the surface of the first intermediate product, and amination modification is carried out to obtain a second intermediate product.
Finally, mixing the second intermediate product with the sodium alginate solution and epoxy chloropropane through the step (5), wherein on one hand, the epoxy chloropropane serving as an etherifying agent can further react with the second intermediate product to modify the surface of the second intermediate product; on the other hand, the sodium alginate has good gel characteristics, the added epoxy chloropropane can generate alcoholic hydroxyl crosslinking reaction with the sodium alginate, and ether bond energy obtained by the crosslinking reaction is stronger than hydrogen bond energy between molecules of the original sodium alginate, so that the viscosity and the heat resistance of the product can be obviously improved.
Therefore, the biomass adsorbent prepared by the method has high viscosity and is not easy to loosen when in use, and is beneficial to recovery; after the prepared biomass adsorbent is modified by sodium acetate, ethylenediamine and epichlorohydrin, the surface of the prepared biomass adsorbent has a large number of active groups such as carboxyl groups, amino groups and the like, the adsorption rate of the biomass adsorbent to dye is greatly improved, the amino groups can be chelated with heavy metal ions, and the adsorption performance of the biomass adsorbent to the heavy metal ions in the printing and dyeing wastewater is improved. Meanwhile, the peanut shells serving as the raw materials are a natural, environment-friendly and economic adsorbent source, have the advantages of rich resources, easiness in obtaining, renewable utilization, low price and the like, and can achieve the purpose of treating wastes with processes of wastes against one another.
Preferably, the concentration of the sodium hydroxide solution in the step (2) is 1-2mol/L, and the swelling time is 3-5 h. Different concentrations of alkali react with cellulose to form crystal modifications with different structures, which have a very different effect on adsorption performance. The concentration of sodium hydroxide is too low, which causes incomplete removal of lignin and lipid, insufficient expansion of cellulose and small specific surface area of the adsorbent; the cellulose is subjected to an infinite swelling phenomenon due to too high alkali concentration, so that the cellulose is dissolved, and the subsequent modification is influenced. Therefore, the biomass adsorbent prepared by adopting the sodium hydroxide concentration and the swelling time for swelling has the best adsorption performance.
Preferably, the adding proportion of the peanut shell powder, the acetic anhydride and the N, N-dimethylformamide in the step (3) is 1g (3-4g) to (30-40 mL). By adopting the proportion of the solvent to the reactant, the acetic anhydride can be fully dissolved, the peanut shell powder and the acetic anhydride can be ensured to fully react, and the surface of the peanut shell powder can be effectively modified.
Preferably, the reaction time in step (3) is 2 to 4 hours. The peanut shell powder and the acetic anhydride can fully react in the reaction time to obtain a first intermediate product, and the adsorption performance and subsequent modification of the adsorbent are improved.
Preferably, in the ethylenediamine aqueous solution in the step (4), the volume ratio of ethylenediamine to water is 1: (9-11). By using the aqueous solution of ethylenediamine with such a concentration, the amination reaction of ethylenediamine with the first intermediate product can be more easily performed.
Preferably, the ratio of the first intermediate product added in step (4) to ethylenediamine added in the aqueous ethylenediamine solution is 1g: (1-2 mL). By adopting the adding proportion of the invention, the first intermediate product can be ensured to fully react with the ethylenediamine, and a proper amount of amino is introduced on the surface of the first intermediate product, so as to improve the adsorption performance of the adsorbent on the dye and heavy metal ions.
Preferably, the stirring reaction time in step (4) is 1 to 3 hours. In the reaction time, the amination reaction can be fully performed.
Preferably, the mass ratio of the sodium alginate to the water in the sodium alginate solution in the step (5) is 1: (10-15). The epichlorohydrin and the water have side reaction, and the large amount of water is not beneficial to the occurrence of crosslinking reaction, so that the proportion in the invention not only ensures that the epichlorohydrin can be fully crosslinked with the sodium alginate, but also can reduce the occurrence of side reaction as much as possible.
Preferably, the adding ratio of the second intermediate product in the step (5) to the sodium alginate and the epichlorohydrin in the sodium alginate solution is 1g (1-3g) to (1-2 mL). By adopting the proportion, the etherification reaction of the second intermediate product and the epoxy chloropropane can be ensured, the surface modification of the second intermediate product can be further carried out, the sufficient crosslinking of the epoxy chloropropane and the sodium alginate can be ensured, the viscosity of the biomass adsorbent is improved, and the adsorbent is not easy to loosen.
Preferably, the reaction time in step (5) is 30 to 60 min. In the reaction time, the second intermediate product and the sodium alginate can fully react with the epichlorohydrin, so that the adsorption performance and the viscosity of the adsorbent are improved.
Therefore, the invention has the following beneficial effects:
(1) the biomass adsorbent prepared by the method has high viscosity and is not easy to loosen when in use, thereby being beneficial to recovery; after the prepared biomass adsorbent is modified by sodium acetate, ethylenediamine and epichlorohydrin, the surface of the prepared biomass adsorbent has a large number of active groups such as carboxyl groups, amino groups and the like, so that the adsorption rate of the biomass adsorbent to dye is greatly improved, the amino groups can be chelated with heavy metal ions, and the adsorption performance of the biomass adsorbent to the heavy metal ions in the printing and dyeing wastewater is improved;
(2) the peanut shells serving as the raw materials are a natural, environment-friendly and economic adsorbent source, have the advantages of rich resources, easiness in obtaining, renewable utilization, low price and the like, and can achieve the purpose of treating wastes with processes of wastes against one another.
Drawings
FIG. 1 is a standard curve of reactive Brilliant Red X-3B;
FIG. 2 is a standard curve of active light yellow X-6G.
Detailed Description
The invention is further described with reference to the following detailed description and accompanying drawings.
Example 1:
(1) soaking peanut shells in water, washing, removing soil and impurities, washing with distilled water, drying at 80 ℃ to constant weight, pulverizing, sieving, and collecting 80-100 mesh granules to obtain peanut shell powder;
(2) immersing the peanut shell powder into 1.5mol/L sodium hydroxide solution for swelling for 4 hours;
(3) adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting for 3 hours at 75 ℃ to obtain a first intermediate product, wherein the adding ratio of the peanut shell powder to the acetic anhydride to the N, N-dimethylformamide is 1g:3.5g:35 mL;
(4) adding the first intermediate product into ethylene diamine and water at a volume ratio of 1: 10, stirring and reacting at 85 ℃ for 2h to obtain a second intermediate product, wherein the adding ratio of the first intermediate product to the ethylenediamine is 1g: 1.5 mL;
(5) and (3) setting the mass ratio of the second intermediate product to sodium alginate to water as 1: 12, adding epichlorohydrin, wherein the adding proportion of the second intermediate product, the sodium alginate and the epichlorohydrin is 1g:2g:1.5mL, reacting at 55 ℃ for 40min, filtering the product, and drying at 60 ℃ for 2h to obtain the biomass adsorbent.
Example 2:
(1) soaking peanut shells in water, washing, removing soil and impurities, washing with distilled water, drying at 80 ℃ to constant weight, pulverizing, sieving, and collecting 80-100 mesh granules to obtain peanut shell powder;
(2) immersing the peanut shell powder into 1mol/L sodium hydroxide solution for swelling for 5 hours;
(3) adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting for 4 hours at 65 ℃ to obtain a first intermediate product, wherein the adding ratio of the peanut shell powder to the acetic anhydride to the N, N-dimethylformamide is 1g:3g:30 mL;
(4) adding the first intermediate product into ethylene diamine and water at a volume ratio of 1: 9, stirring and reacting at 80 ℃ for 3h to obtain a second intermediate product, wherein the adding ratio of the first intermediate product to the ethylenediamine is 1g:1 mL;
(5) and (3) setting the mass ratio of the second intermediate product to sodium alginate to water as 1: 10, then adding epichlorohydrin, wherein the adding proportion of the second intermediate product, the sodium alginate and the epichlorohydrin is 1g:1g:1mL, reacting at 50 ℃ for 60min, filtering the product, and drying at 60 ℃ for 2h to obtain the biomass adsorbent.
Example 3:
(1) soaking peanut shells in water, washing, removing soil and impurities, washing with distilled water, drying at 80 ℃ to constant weight, pulverizing, sieving, and collecting 80-100 mesh granules to obtain peanut shell powder;
(2) immersing the peanut shell powder into a 2mol/L sodium hydroxide solution for swelling for 3 h;
(3) adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting at 85 ℃ for 2 hours to obtain a first intermediate product, wherein the adding ratio of the peanut shell powder to the acetic anhydride to the N, N-dimethylformamide is 1g:4g:40 mL;
(4) adding the first intermediate product into ethylene diamine and water at a volume ratio of 1: 11, stirring and reacting at 90 ℃ for 1h to obtain a second intermediate product, wherein the adding ratio of the first intermediate product to the ethylenediamine is 1g:2 mL;
(5) and (3) setting the mass ratio of the second intermediate product to sodium alginate to water as 1: 15, adding epichlorohydrin, wherein the adding proportion of the second intermediate product, the sodium alginate and the epichlorohydrin is 1g:3g:2mL, reacting at 60 ℃ for 30min, filtering the product, and drying at 60 ℃ for 2h to obtain the biomass adsorbent.
Comparative example 1:
soaking peanut shells in water, washing, removing soil and impurities, washing with distilled water, drying at 80 ℃ to constant weight, crushing and sieving, and taking particles with the size of 80-100 meshes to obtain peanut shell powder serving as a biomass adsorbent.
Comparative example 2:
(1) soaking peanut shells in water, washing, removing soil and impurities, washing with distilled water, drying at 80 ℃ to constant weight, pulverizing, sieving, and collecting 80-100 mesh granules to obtain peanut shell powder;
(2) immersing the peanut shell powder into 1.5mol/L sodium hydroxide solution for swelling for 4 hours;
(3) and (3) mixing the swelled peanut shell powder with sodium alginate and water in a mass ratio of 1: 12, adding epoxy chloropropane, the adding proportion of the peanut shell powder to the sodium alginate to the epoxy chloropropane is 1g to 2g to 1.5mL, reacting at 55 ℃ for 40min, and filtering to obtain a first intermediate product;
(4) adding the first intermediate product into N, N-dimethylformamide dissolved with acetic anhydride, and reacting at 75 ℃ for 3h to obtain a second intermediate product, wherein the adding ratio of the first intermediate product to the acetic anhydride to the N, N-dimethylformamide is 1g:3.5g:35 mL;
(5) adding the second intermediate product into the mixture of ethylenediamine and water in a volume ratio of 1: 10 of ethylenediamine aqueous solution, wherein the adding ratio of the second intermediate product to ethylenediamine is 1g: 1.5mL, stirring and reacting at 85 ℃ for 2h, filtering the product, and drying at 60 ℃ for 2h to obtain the biomass adsorbent.
Comparative example 3:
comparative example 3 is different from example 1 in that the addition ratio of the peanut shell powder, acetic anhydride and N, N-dimethylformamide in step (3) is 1g:2g:35 mL.
Comparative example 4:
comparative example 4 differs from example 1 in that the addition ratio of the first intermediate product to ethylenediamine in step (4) was 1g: 0.5 mL.
Comparative example 5:
comparative example 5 differs from example 1 in that the addition ratio of the second intermediate product, sodium alginate and epichlorohydrin in step (5) was 1g:3g:0.5 mL.
The biomass adsorbents prepared in the above examples and comparative examples were used to perform adsorption experiments on reactive bright red X-3B and reactive bright yellow X-6G dyes, and the adsorption effects thereof were studied. The method comprises the following steps: accurately transferring 50mL of reactive bright red X-3B and reactive bright yellow X-6G dye solutions with certain concentrations into a 250mL conical flask, adding a certain mass of biomass adsorbent, placing the conical flask into a constant-temperature oscillator, oscillating for a certain time to reach adsorption balance, filtering, measuring the absorbance of filtrate at the maximum absorption wavelength of the dye (the reactive bright red X-3B: 538 nm; the reactive bright yellow X-6G: 420nm) by using a visible spectrophotometer, calculating the concentration of the solution after adsorption according to a standard curve of the corresponding dye, and then respectively calculating the adsorption capacity and the decolorization rate of the biomass adsorbent to the reactive bright red X-3B and the reactive bright yellow X-6G.
The adsorption amount calculation formula is as follows:
adsorption capacity q at equilibriume：
Decolorization ratio η:
in the formula qe(mg/g) represents an adsorption amount at adsorption equilibrium; c. C0(mg/L) represents the initial concentration of the solution; c. Ce(mg/L) represents the adsorption equilibrium liquid phase concentration; v (L) represents the volume of the adsorption solution; w (g) represents the mass of the adsorbent; eta (%) indicates the decolorization rate of the dye by the adsorbent.
The reactive brilliant red solution used by the invention is obtained by diluting a reactive brilliant red X-3B stock solution, and the preparation method of the reactive brilliant red X-3B stock solution comprises the following steps: accurately weighing 1.000g of reactive brilliant red X-3B dye by using an analytical balance, fully stirring and dissolving the dye by using distilled water and a glass rod, transferring the dye into a 1000mL volumetric flask, then fixing the volume to a scale mark by using the distilled water, fully shaking up, preparing a stock solution of 1000mg/L, and preparing the stock solution into a required concentration according to a proportion when in use.
The active light yellow solution used by the invention is obtained by diluting an active light yellow X-6G stock solution, and the preparation method of the active light yellow X-6G stock solution comprises the following steps: accurately weighing 1.000G of active light yellow X-6G dye by using an analytical balance, fully stirring and dissolving the dye by using distilled water and a glass rod, transferring the dye into a 1000mL volumetric flask, then fixing the volume to a scale mark by using the distilled water, fully shaking up to prepare 1000mg/L stock solution, and preparing the stock solution into the required concentration according to the proportion when in use.
And (3) drawing a reactive brilliant red X-3B standard curve:
0, 1, 3, 4, 5, 6, 7mL of reactive brilliant red standard stock solution were transferred into volumetric flasks, diluted to 100mL of the standard line with distilled water, shaken up, and the absorbance was measured at 538nm using a 1cm cuvette with distilled water as a reference, the results of which are shown in Table 1. From the obtained data, a standard curve was prepared with the concentration of the solution as the abscissa and the absorbance as the ordinate, as shown in FIG. 1.
TABLE 1 reactive Brilliant Red X-3B Standard Curve.
| Group of | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Stock volume V (mL) | 0 | 1 | 3 | 4 | 5 | 6 | 7 |
| Concentration of solution c (mg/L) | 0 | 10 | 30 | 40 | 50 | 60 | 70 |
| Absorbance A | 0.003 | 0.158 | 0.434 | 0.605 | 0.759 | 0.912 | 1.040 |
And (3) drawing an active light yellow X-6G standard curve:
0, 1, 3, 5, 8, 10, 12mL of reactive brilliant red standard stock solution was transferred to a volumetric flask, diluted to 100mL of a standard line with distilled water, shaken up, and measured for absorbance at a wavelength of 420nm using a 1cm cuvette with distilled water as a reference, with the results shown in Table 2. From the obtained data, a standard curve was prepared with the concentration of the solution as the abscissa and the absorbance as the ordinate, as shown in FIG. 2.
TABLE 2 reactive light yellow X-6G standard curve.
| Group of | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Stock volume V (mL) | 0 | 1 | 3 | 5 | 8 | 10 | 12 |
| Concentration of solution c (mg/L) | 0 | 10 | 30 | 50 | 80 | 100 | 120 |
| Absorbance A | 0.002 | 0.088 | 0.256 | 0.427 | 0.642 | 0.812 | 0.966 |
Firstly, the influence of the dosage of the biomass adsorbent on the decoloring effect of two reactive dyes:
1. influence of biomass adsorbent dosage on decolorizing effect of active brilliant red X-3B
50mL of active brilliant red X-3B solution with the initial concentration of 60mg/L is accurately transferred into seven 250mL conical flasks, biomass adsorbents prepared in the example 1 with the mass of 0.2, 0.4, 0.6, 0.8, 1.0, 1.2 and 1.4g are respectively added, the rotating speed is set at 120r/min at normal temperature, the biomass adsorbents are oscillated for 40min at constant temperature, the biomass adsorbents are subjected to suction filtration, the absorbance of filtrate is measured under a visible spectrophotometer, and the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 3.
TABLE 3 impact of biomass adsorbent dosage on reactive bright red X-3B.
| Mass (g) of biomass adsorbent | 0.2 | 0.4 | 0.6 | 0.8 | 1.0 | 1.2 | 1.4 |
| Concentration of solution ce(mg/L) | 31.728 | 16.117 | 11.114 | 8.846 | 5.777 | 4.710 | 4.510 |
| Decolorization rate eta% | 47.70 | 73.36 | 81.58 | 85.30 | 90.35 | 92.11 | 93.37 |
| Adsorption capacity qe(mg/g) | 7.068 | 5.485 | 4.074 | 3.197 | 2.711 | 2.304 | 1.982 |
As can be seen from Table 3, when the initial concentration of the reactive brilliant red X-3B is 60mg/L, the dosage of the adsorbent is between 0.2 and 1.4g, the decolorization rate of the dye is higher and higher with the increase of the dosage of the adsorbent, and when the dosage of the adsorbent is about 1g, the removal rate tends to be balanced, and the removal effect is the best.
2. Influence of biomass adsorbent dosage on decolorization effect of active light yellow X-6G
50mL of active light yellow X-6G solution with the initial concentration of 120mg/L is accurately transferred into seven 250mL conical flasks, 0.2, 0.4, 0.6, 0.8, 0.9, 1.0 and 1.2G of the biomass adsorbent prepared in the example 1 are respectively added, the rotating speed is set at 120r/min at normal temperature, the constant temperature oscillation is carried out for 50min, the filtration is carried out, the absorbance of the filtrate is measured under a visible spectrophotometer, the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 4.
TABLE 4 Effect of Biomass adsorbent dosage on active Bright yellow X-6G
| Mass (g) of biomass adsorbent | 0.2 | 0.4 | 0.6 | 0.8 | 0.9 | 1.0 | 1.2 |
| Concentration of solution ce(mg/L) | 66.625 | 42.875 | 32.250 | 16.000 | 15.375 | 15.125 | 14.875 |
| Decolorization rate eta% | 43.79 | 63.46 | 72.26 | 85.71 | 86.23 | 86.44 | 86.65 |
| Adsorption capacity qe(mg/g) | 13.344 | 9.641 | 7.313 | 6.500 | 5.813 | 5.244 | 4.380 |
As can be seen from Table 4, when the initial concentration of the active light yellow X-6G is 120mg/L, the dosage of the adsorbent is between 0.2 and 1.2G, the decoloring rate of the dye is higher and higher with the increase of the dosage of the adsorbent, and when the dosage of the adsorbent is about 0.8G, the removal rate tends to be balanced, and the removal effect is the best.
Secondly, the influence of the initial concentration of the solution on the decoloring effect of the two reactive dyes
1. Effect of initial concentration of solution on decolorization Effect of reactive Brilliant Red X-3B
50mL of active brilliant red X-3B with initial concentrations of 30, 40, 50, 6, 70 and 80mg/L is accurately transferred into six 250mL conical flasks, 1g of the biomass adsorbent prepared in example 1 is added into each flask, the rotating speed is set at 120r/min at normal temperature, the mixture is subjected to constant temperature oscillation for 40min, suction filtration is carried out, the filtrate is subjected to absorbance measurement under a visible spectrophotometer, and the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 5.
TABLE 5 influence of initial concentration of the solution on the adsorption effect of reactive bright red X-3B.
| Initial concentration (mg/L) | 30 | 40 | 50 | 60 | 70 | 80 |
| Concentration of solution ce(mg/L) | 0.507 | 0.907 | 2.108 | 5.644 | 10.047 | 16.184 |
| Decolorization rate eta% | 98.31 | 97.73 | 95.78 | 90.59 | 85.65 | 79.77 |
| Adsorption capacity qe(mg/g) | 1.475 | 1.955 | 2.395 | 2.718 | 2.998 | 3.191 |
As can be seen from Table 5, under the condition of constant temperature, adsorbent dosage and the like, the decolorization rate of the adsorbent to the active brilliant red X-3B solution is continuously reduced along with the continuous increase of the initial concentration, and the decolorization rate is maximized when the initial concentration is 30 mg/L. This is because the binding sites between the dye and the adsorbent are constant when the amount of the dye is constant, and the unbound sites in the dye increase as the concentration of the dye solution increases, and the ratio of the bound sites increases, thereby showing a decrease in the decolorization rate.
2. Influence of initial concentration of solution on decolorization effect of active light yellow X-6G
50mL of active light yellow X-6G with initial concentration of 60, 90, 120, 150, 180 and 210mg/L is accurately transferred into six conical flasks of 250mL, 0.8G of the biomass adsorbent prepared in example 1 is added into each conical flask, the rotating speed is set at 120r/min at normal temperature, the conical flasks are oscillated at constant temperature for 50min, the filtering is carried out, the absorbance of the filtrate is measured under a visible spectrophotometer, and the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 6.
TABLE 6 influence of initial concentration of the solution on the adsorption effect of active light yellow X-6G.
| Initial concentration (mg/L) | 60 | 90 | 120 | 150 | 180 | 210 |
| Concentration of solution ce(mg/L) | 3.000 | 6.750 | 15.250 | 26.625 | 42.875 | 64.625 |
| Decolorization rate eta% | 95.00 | 92.50 | 87.29 | 82.25 | 76.18 | 69.23 |
| Adsorption capacity qe(mg/g) | 3.563 | 5.203 | 6.547 | 7.711 | 8.570 | 9.086 |
As can be seen from Table 6, under the condition of no change in temperature, the amount of the adsorbent and the like, the decolorization rate of the adsorbent to the active light yellow X-6G solution is continuously reduced along with the continuous increase of the initial concentration, and the decolorization rate is maximized when the initial concentration is 60 mg/L.
Influence of solution pH on decoloring effect of two reactive dyes
1. Effect of solution pH on decolorizing Effect of reactive Brilliant Red X-3B
50mL of active brilliant red X-3B solution with the initial concentration of 60mg/L is accurately transferred into six 250mL conical flasks, the pH value of the dye solution is adjusted to 1, 2, 3, 4, 5 and 6 by using 1moL/L hydrochloric acid, 1g of the biomass adsorbent prepared in the example 1 is added respectively, the rotating speed is set at 120r/min at normal temperature, the constant temperature oscillation is carried out for 40min, the filtration is carried out, the absorbance of the filtrate is measured under a visible spectrophotometer, the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 7.
TABLE 7 influence of solution pH on the adsorption effect of reactive Brilliant Red X-3B.
| pH of the |
1 | 2 | 3 | 4 | 5 | 6 |
| Concentration of solution ce(mg/L) | 5.043 | 5.310 | 5.777 | 10.180 | 37.799 | 45.404 |
| Decolorization rate eta% | 91.56 | 91.12 | 90.35 | 83.11 | 37.72 | 25.22 |
| Adsorption capacity qe(mg/g) | 2.748 | 2.734 | 2.711 | 2.491 | 1.110 | 0.730 |
As can be seen from Table 7, pH has a large influence on the adsorption performance of the biomass adsorbent on the reactive bright red X-3B. In the pH range of 1-4, the adsorbent has obvious adsorption effect on dye, the decolorization rate can reach more than 83%, the unit adsorption capacity can reach more than 2.49mg/g, the dye adsorption performance is good, the pH is between 1 and 3, and the decolorization rate of the adsorbent on active brilliant red X-3B is about 90%; however, when the pH value is increased, the decolorization rate of the adsorbent to the active brilliant red X-3B is obviously reduced, the decolorization rate is rapidly reduced from 83.1% to 25.2% when the pH value is between 4 and 6, and the condition that the pH value is more than or equal to 7 is not discussed because the active brilliant red X-3B is faintly acid, the pH value is about 6 and the color is changed under the alkaline condition. Therefore, the pH of the reactive bright red X-3B solution in the subsequent experiment is adjusted to 3. The decolorization rate can vary greatly with pH, and it is likely that the adsorption capacity of the adsorbent for reactive bright red X-3B is greatly reduced due to the drastic decrease of the surface functional groups of the adsorbent with the increase of pH.
2. Influence of solution pH on decolorization effect of active light yellow X-6G
50mL of active light yellow X-6G solution with the initial concentration of 120mg/L is accurately transferred into six conical flasks of 250mL, the pH of the dye solution is adjusted to 1, 2, 3, 4, 5 and 6 by using 1moL/L hydrochloric acid, 0.8G of the biomass adsorbent prepared in the example 1 is added respectively, the rotating speed is set at 120r/min at normal temperature, the constant temperature oscillation is carried out for 50min, the filtration is carried out, the absorbance of the filtrate is measured under a visible spectrophotometer, the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 8.
TABLE 8 influence of solution pH on the adsorption effect of active light yellow X-6G.
| pH of the |
1 | 2 | 3 | 4 | 5 | 6 |
| Concentration of solution ce(mg/L) | 11.375 | 12.875 | 19.250 | 25.750 | 38.875 | 82.625 |
| Decolorization rate eta% | 89.54 | 88.30 | 83.02 | 77.64 | 66.77 | 30.54 |
| Adsorption capacity qe(mg/g) | 6.789 | 6.695 | 6.297 | 5.891 | 5.070 | 2.336 |
As can be seen from Table 8, pH had a large influence on the adsorption performance of active light yellow X-6G. In the pH range of 1-5, the adsorbent has obvious adsorption effect on dye, the decolorization rate can reach more than 66.8 percent, the unit adsorption capacity can reach more than 5.07mg/G, the dye adsorption performance is good, the pH is between 1 and 2, and the decolorization rate of the adsorbent on active light yellow X-6G is about 90 percent; however, when the pH value is increased, the decolorization rate of the adsorbent to the active light yellow X-6G is obviously reduced, the decolorization rate is rapidly reduced from 66.8% to 30.5% when the pH value is between 5 and 6, and because the active light yellow X-6G is in subacidity, the pH value is about 6, and the color is changed under the alkaline condition, so that the condition that the pH value is more than or equal to 7 is not discussed. Therefore, the pH of the active light yellow X-6G solution in the subsequent experiments was adjusted to 2.
Fourth, the influence of the oscillation adsorption temperature on the decoloring effect of the two reactive dyes
1. Influence of oscillatory adsorption temperature on decolorizing effect of active brilliant red X-3B
50mL of active bright red X-3B solution with the initial concentration of 60mg/L is accurately transferred into six 250mL conical flasks, 1g of the biomass adsorbent prepared in example 1 is added into each flask, different adsorption temperatures are set, the flasks are placed in a constant-temperature oscillation incubator at the temperatures of 10, 15, 20, 25, 30 and 40 ℃, the rotation speed is set to be 120r/min, the flasks are subjected to constant-temperature oscillation for 50min, the filtration is carried out, the absorbance of the filtrate is measured under a visible spectrophotometer, and the decolorization rate and the adsorption amount are calculated, and the results are shown in Table 9.
TABLE 9 influence of the shaking adsorption temperature on the adsorption effect of reactive bright red X-3B.
| Adsorption temperature (. degree.C.) | 10 | 15 | 20 | 25 | 30 | 40 |
| Concentration of solution ce(mg/L) | 5.043 | 5.977 | 7.445 | 8.179 | 8.512 | 9.046 |
| Decolorization rate eta% | 91.56 | 90.02 | 87.61 | 86.40 | 85.86 | 84.98 |
| Adsorption capacity qe(mg/g) | 2.748 | 2.701 | 2.628 | 2.591 | 2.574 | 2.548 |
2. Influence of oscillating adsorption temperature on decolorizing effect of active light yellow X-6G
50mL of active light yellow X-6G solution with the initial concentration of 120mg/L is accurately transferred into six 250mL conical flasks, 0.8G of the biomass adsorbent prepared in example 1 is added into each flask, different adsorption temperatures are set, the flasks are placed in a constant-temperature oscillation incubator at the temperatures of 10 ℃, 15 ℃, 20, 25, 30 and 40 ℃, the rotation speed is set to be 120r/min, the flasks are subjected to constant-temperature oscillation for 50min, the flasks are subjected to suction filtration, the filtrate is subjected to absorbance measurement under a visible spectrophotometer, and the decolorization rate and the adsorption amount are calculated, and the results are shown in Table 10.
TABLE 10 influence of the Oscillating adsorption temperature on the adsorption Effect of active Bright yellow X-6G
| Adsorption temperature (. degree.C.) | 10 | 15 | 20 | 25 | 30 | 40 |
| Concentration of solution ce(mg/L) | 10.375 | 12.750 | 14.125 | 15.500 | 16.125 | 17.125 |
| Decolorization rate eta% | 90.37 | 88.41 | 87.27 | 86.13 | 85.61 | 84.78 |
| Adsorption capacity qe(mg/g) | 6.852 | 6.703 | 6.617 | 6.531 | 6.492 | 6.430 |
As can be seen from tables 9 and 10, under the condition that the initial concentrations of the reactive brilliant red X-3B and the reactive bright yellow X-6G are respectively 60mg/L and 120mg/L, and other single-factor factors are not changed, the decoloring rate and the adsorption amount of the two reactive dyes are slightly reduced along with the increase of the oscillating adsorption temperature. This is probably because the adsorption of the biomass adsorbent to the two reactive dyes is mainly physical adsorption and belongs to exothermic reaction, and the reaction is not favored by the temperature rise.
Fifthly, influence of oscillation adsorption time on decoloring effect of two reactive dyes
1. Influence of oscillatory adsorption time on decolorizing effect of active brilliant red X-3B
50mL of active bright red X-3B solution with the initial concentration of 60mg/L is accurately transferred into six 250mL conical flasks, 1g of the biomass adsorbent prepared in example 1 is added into each flask, different adsorption times are set, the adsorption time is respectively 20, 30, 40, 60, 90 and 120min, the rotation speed is set to be 120r/min, the mixture is subjected to constant temperature oscillation and suction filtration, the filtrate is subjected to absorbance measurement under a visible spectrophotometer, the decolorization rate and the adsorption quantity are calculated, and the results are shown in Table 11.
TABLE 11 influence of shaking adsorption time on the adsorption effect of reactive bright red X-3B.
| Adsorption time t (min) | 20 | 30 | 40 | 60 | 90 | 120 |
| Concentration of solution ce(mg/L) | 10.380 | 7.178 | 5.710 | 5.577 | 5.510 | 5.510 |
| Decolorization rate eta% | 82.79 | 88.05 | 90.46 | 90.68 | 90.79 | 90.79 |
| Adsorption capacity qe(mg/g) | 2.481 | 2.641 | 2.714 | 2.721 | 2.724 | 2.724 |
2. Influence of oscillation adsorption time on decolorizing effect of active light yellow X-6G
50mL of active light yellow X-6G solution with the initial concentration of 120mg/L is accurately transferred into six 250mL conical flasks, 0.8G of the biomass adsorbent prepared in the example 1 is added into each flask, the flasks are placed in a constant-temperature shaking incubator at room temperature, the rotation speed is 120r/min, the biomass adsorbent is adsorbed for 20min, 30min, 40min, 50min, 90 min and 120min respectively, the biomass adsorbent is subjected to suction filtration, the filtrate is subjected to absorbance measurement under a visible spectrophotometer, the decolorization rate and the adsorption amount are calculated, and the results are shown in Table 12.
TABLE 12 influence of shaking adsorption time on the adsorption effect of active light yellow X-6G.
| Adsorption time t (min) | 20 | 30 | 40 | 50 | 90 | 120 |
| Concentration of solution ce(mg/L) | 30.875 | 17.375 | 12.875 | 12.625 | 12.250 | 12.250 |
| Decolorization rate eta% | 73.40 | 84.58 | 88.30 | 88.51 | 88.82 | 88.82 |
| Adsorption capacity qe(mg/g) | 5.570 | 6.414 | 6.695 | 6.711 | 6.734 | 6.734 |
As can be seen from tables 11 and 12, under the condition that each single factor is unchanged, the decolorization rate and the adsorption amount of the two reactive dyes are increased along with the increase of the oscillation adsorption time within 20-50 min; within 50-120min, the decolorization rate and the adsorption capacity of the two reactive dyes tend to be stable, which shows that the adsorption of the biomass adsorbent to the two reactive dyes reaches balance within about 50 min.
Sixthly, the decolorizing effect of different biomass adsorbents on two reactive dyes
1. Decolorizing effect of different biomass adsorbents on active brilliant red X-3B
50mL of active bright red X-3B solution with the initial concentration of 60mg/L is accurately transferred into six 250mL conical flasks, 1g of the biomass adsorbent prepared in each example and comparative example is added into the six conical flasks, the flasks are placed in a constant-temperature shaking incubator at room temperature, the rotation speed is set at 120r/min, the flasks are subjected to constant-temperature shaking for 40min, the filtration is performed, the filtrate is subjected to absorbance measurement under a visible spectrophotometer, and the decolorization rate and the adsorption amount are calculated, and the results are shown in Table 13.
TABLE 13 decolorization effect of different biomass adsorbents on reactive brilliant red X-3B.
2. Decolorizing effect of different biomass adsorbents on active light yellow X-6G
50mL of active light yellow X-6G solution with the initial concentration of 120mg/L is accurately transferred into six 250mL conical flasks, 0.8G of the biomass adsorbent prepared in each example and comparative example is added into the six conical flasks, the flasks are placed in a constant-temperature shaking incubator at room temperature, the rotating speed is 120r/min, the constant-temperature shaking incubator is subjected to 50min, the filtration is performed, the filtrate is subjected to suction filtration, the absorbance is measured under a visible spectrophotometer, the decolorization rate and the adsorption amount are calculated, and the results are shown in Table 14.
TABLE 14 decolorization effect of different biomass adsorbents on reactive brilliant red X-3B.
As can be seen from tables 13 and 14, the biomass adsorbents obtained in examples 1 to 3 by the method of the present invention have good adsorption properties for both dyes. While comparative example 1 does not modify the peanut shell powder and is used directly as a biomass adsorbent; comparative example 2 the order of modification was changed; comparative examples 3 to 5 the amount of the reactants used in the modification was changed to fall outside the scope of the present invention, and the adsorption performance of the biomass adsorbent obtained was significantly reduced for both fuels as compared with example 1. The order of modification and the amounts of reactants in the steps of the present invention prove to be an unconventional choice.
Claims (10)
1. A preparation method of a biomass adsorbent for printing and dyeing wastewater treatment is characterized by comprising the following steps:
(1) cleaning peanut shells, drying, crushing and sieving to obtain peanut shell powder;
(2) putting the peanut shell powder into a sodium hydroxide solution for swelling;
(3) adding the swelled peanut shell powder into N, N-dimethylformamide dissolved with acetic anhydride, and reacting at 65-85 ℃ to obtain a first intermediate product;
(4) adding the first intermediate product into an ethylene diamine aqueous solution, and stirring and reacting at 80-90 ℃ to obtain a second intermediate product;
(5) and uniformly mixing the second intermediate product with a sodium alginate solution, adding epoxy chloropropane, reacting at 50-60 ℃, filtering and drying the product to obtain the biomass adsorbent.
2. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1, characterized in that the concentration of the sodium hydroxide solution in the step (2) is 1-2mol/L, and the swelling time is 3-5 h.
3. The method for preparing the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1, wherein the peanut shell powder, the acetic anhydride and the N, N-dimethylformamide are added in a ratio of 1g (3-4g) to 30-40mL in step (3).
4. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1 or 3, characterized in that the reaction time in step (3) is 2-4 h.
5. The method for preparing the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1, wherein the volume ratio of ethylenediamine to water in the ethylenediamine aqueous solution in the step (4) is 1: (9-11).
6. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1 or 5, characterized in that the adding ratio of the first intermediate product added in the step (4) to the ethylenediamine in the ethylenediamine aqueous solution is 1g: (1-2 mL).
7. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1 or 5, characterized in that the stirring reaction time in the step (4) is 1-3 h.
8. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment as claimed in claim 1, wherein the mass ratio of sodium alginate to water in the sodium alginate solution in step (5) is 1: (10-15).
9. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment as claimed in claim 1 or 8, wherein the addition ratio of the second intermediate product to the sodium alginate and the epichlorohydrin in the sodium alginate solution in the step (5) is 1g (1-3g) to (1-2 mL).
10. The preparation method of the biomass adsorbent for printing and dyeing wastewater treatment according to claim 1 or 8, characterized in that the reaction time in step (5) is 30-60 min.
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| CN112108111A (en) * | 2020-08-13 | 2020-12-22 | 常熟理工学院 | Porous maple sphere-based biomass charcoal material and application thereof |
| CN112354523A (en) * | 2020-10-11 | 2021-02-12 | 桂林理工大学 | Anhydride modified passion fruit peel biological adsorbent and preparation method and application thereof |
| CN114288996A (en) * | 2022-01-11 | 2022-04-08 | 三明医学科技职业学院 | Preparation method of printing and dyeing sewage treatment agent based on biomass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112108111A (en) * | 2020-08-13 | 2020-12-22 | 常熟理工学院 | Porous maple sphere-based biomass charcoal material and application thereof |
| CN112354523A (en) * | 2020-10-11 | 2021-02-12 | 桂林理工大学 | Anhydride modified passion fruit peel biological adsorbent and preparation method and application thereof |
| CN114288996A (en) * | 2022-01-11 | 2022-04-08 | 三明医学科技职业学院 | Preparation method of printing and dyeing sewage treatment agent based on biomass |
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