CN103566905A - Modified wood chip adsorbent, and preparation method and application thereof in treating wastewater containing basic dye - Google Patents
Modified wood chip adsorbent, and preparation method and application thereof in treating wastewater containing basic dye Download PDFInfo
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Abstract
The invention discloses a modified wood chip adsorbent, and a preparation method and an application of the modified wood chip adsorbent in treating wastewater containing basic dye. The preparation method of the modified wood chip adsorbent comprises the following steps: reacting wood chips with organic acid, drying, subsequently performing an esterification reaction, removing organic acid, and drying to obtain the modified wood chip adsorbent, wherein the organic acid is one or more of oxalic acid, citric acid or tartaric acid. The modified wood chip adsorbent has the characteristics that the materials are simple and easy to obtain, the adsorption quantity is large, the removal rate is high, and the like, and the modified wood chip adsorbent can be applied to treatment on wastewater, especially treatment on alkali dye wastewater; the used raw materials are cheap and easy to obtain, a preparation process is simple, free of pollution, low in cost and easy to industrialize, and the purpose of waste recycling is achieved.
Description
Technical field
The present invention relates to water and pollute process field, specifically relate to a kind of modified wood chips adsorbent, preparation method and the application in water pollution control thereof.
Background technology
Dyestuff is widely used in dyeing industry, as weaving, papermaking, leather, wool and cosmetics etc.According to statistics, without the dyestuff of dealing carefully with regard to being discharged in environment, account for 15% of whole world gross contamination emission.This waste water has that color and luster is dark, stink is large, COD content is high, complicated component and changeable feature, once enter by all means water body environment, will directly or indirectly destroy ecological environment and health be caused to serious harm.Therefore, how effectively to solve the problem of environmental pollution that waste water from dyestuff causes, become focus and difficult point that people pay close attention to.The method of processing at present Wastewater Dyes can be divided into Physical, chemical method and bioanalysis.Because its processing cost is too high, physical-chemical process is difficult to extensive use in practice.And bioanalysis is very limited to the decolored degradation of waste water from dyestuff.Absorption method is because equipment investment is few, and technique and simple to operate, efficient, is with a wide range of applications.For the various feature of kind of dyes in dyeing waste water, that the key of improving absorption method is to find is more efficient, environmental protection, inexpensive sorbing material.
In recent years, a large amount of biological materials cheap and easy to get obtain more research in the processing of waste water from dyestuff as adsorbent.As Chinese patent CN103212378A discloses a kind of preparation method and application thereof of citric acid modification palm bark adsorbent, first palm bark is washed with water and remove earth and impurity, dry, pulverize, after dry with the processing of the NaOH aqueous solution, mix with citric acid solution, cooling after reaction a period of time, be washed with water to without citric acid and exist, with magnesium chloride solution, mix again, suction filtration, dry to obtain adsorbent, the raw material of present patent application is the bark of palm, raw material restriction is stricter, need to make to be soaked in water 7-10 days to remove non-fibrous material, processing time is long, with needing to use NaOH solution to do basification before citric acid treatment, with needing to use magnesium chloride to process after citric acid treatment, complicated process steps, the time is long, with high costs, has limited it and has promoted the use of.
Patent CN102266756A discloses a kind of preparation method and application thereof of citric acid modified rape straw adsorbent, after rape stalk being ground, clean, be dried, need first with isopropyl alcohol, to clean, mixing cleaning-drying with sodium hydroxide solution, finally with citric acid solution, process again, dry after basification, be used for removing positive dyestuff and heavy metal ion in waste water, the art of this patent route is complicated, and use poisoning isopropyl alcohol, easily cause secondary pollution.
Patent CN101474816A discloses a kind of method of preparation and use of modified wood chips, has used the organic substances such as Isosorbide-5-Nitrae-dioxane, chloropropylene oxide, monosodium glutamate in the preparation method of its wood chip, and route is complicated, with high costs.Gong Xinhuai etc., have studied citric acid-modified bamboo bits absorption methylene blue, and its maximum adsorption capacity is 125mg/g, (Gong Xinhuai etc., dynamics and the thermodynamic analysis of citric acid-modified bamboo bits absorption methylene blue, Yichun College's journal, 2012,34 (8), 47～49).These agricultural refuses have the advantages such as renewable, degradable as the adsorbent of wastewater treatment, are important living resources, but the drawbacks limit such as adsorption capacity is low, manufacturing cost is high, raw material sources are limited being widely used of they.
Summary of the invention
The object of this invention is to provide a kind of modified wood chips adsorbent, its adsorption capacity is large, high to the basic-dyeable fibre clearance in waste water, the present invention also provides the preparation method of modified wood chips adsorbent, its route is simple, low cost of manufacture, to environment non-secondary pollution, the present invention also provides described modified wood chips adsorbent processing containing the application in basic-dyeable fibre waste water.
The invention provides a kind of modified wood chips adsorbent, preparation method is as follows: take wood chip as raw material, with organic acid reaction, after dry, carry out esterification, remove organic acid, dry, obtain modified wood chips adsorbent, described organic acid is one or more in oxalic acid, citric acid or tartaric acid.
Specifically comprise the steps:
1, by wood chip cleaning, oven dry, grinding and sieving, then wood chip is added in organic acid soln, under room temperature, mix, described wood chip is preferably camphorwood dust, and described organic acid soln is one or more in oxalic acid, citric acid or tartaric acid solution, and concentration is preferably 1.0～1.2mol/L, the mass volume ratio of wood chip and organic acid soln is preferably 40～60g/L, hybrid mode is preferably and stirs or concussion mode, and the speed of concussion mode is 200rpm, and the time is 3 hours.
2, stir and finish rear Separation of Solid and Liquid, wood chip solid is dried, baking temperature is preferably 50-70 ℃, and the time is 24 hours.
3, be warming up to 110～120 ℃, carry out esterification, continue 80～120min, the principle of esterification is that organic acid sticks to wood chip surface by physical action, the dry rear moisture of removing, wood chip and organic acid generation esterification after then heating up.
4, be cooled to after room temperature, utilize alkaline solution repeatedly to clean, the preferred sodium acid carbonate of alkaline solution or potassium bicarbonate solution, concentration is 0.05mol/L, until in filtrate without organic acid, can adopt 0.1mol/L lead nitrate solution to detect this filtrate.
5, be dried and sieve, obtaining modified wood chips adsorbent, preferable particle size is 45～75mm.
The present invention also provides a kind of modified wood chips adsorbent in the application of processing water pollution field, step is, modified wood chips adsorbent prepared by above-mentioned preparation method joins in the waste water that contains basic-dyeable fibre, described basic-dyeable fibre is preferably malachite green dyestuff or methylene blue dye, addition is 0.2-10g/L, adopt mechanical agitation or concussion mode to mix, the preferred rotating speed of concussion mode is 170rpm, temperature is 30-40 ℃, time is 3-24 hour, carry out after completion of the reaction Separation of Solid and Liquid, isolate the adsorbent of load basic-dyeable fibre.
The present invention has following beneficial effect: (1) wood raw material is easy to get; (2) preparation technology is simple, does not have to use the material that environment is had to harm, can not produce secondary pollution to environment, with low cost, is suitable for the batch production of continuous large-scale; (3) modified wood chips adsorbent has porous, permeability, specific area is large and contain a large amount of chemical functional groups, as carboxyl, can form various bonding forces with dyestuff, as ion-exchange, electrostatic attraction and hydrogen bond etc., is beneficial to the pollution of processing in waste water.(4) modified wood chips adsorbent of the present invention is high to the clearance of basic-dyeable fibre, and capacity is large, and use amount is little.
Accompanying drawing explanation
Fig. 1 is the ESEM contrast figure of different camphorwood dusts.
Wherein, (a) being camphorwood dust, is (b) that oxalic acid modification camphorwood dust, (c) are citric acid-modified camphorwood dust, (d) is tartaric acid modification camphorwood dust.
Fig. 2 is the infrared spectrum contrast figure of different camphorwood dusts.
Wherein, (a) being camphorwood dust, is (b) that oxalic acid modification camphorwood dust, (c) are citric acid-modified camphorwood dust, (d) is tartaric acid modification camphorwood dust.
Fig. 3 is the clearance schematic diagram of the modified wood chips Adsorbent For Removal of Heavy Malachite Green dyestuff of different amounts.
Fig. 4 is modified wood chips adsorbent clearance schematic diagram to waste water Malachite Green dyestuff under different pH condition.
Fig. 5 is the modification camphorwood dust adsorbent of the different initial concentrations adsorbance schematic diagram to malachite green dyestuff.
The specific embodiment
Below by specific embodiment, the present invention will be described in more detail.Embodiment is only to a kind of explanation of the present invention, and is not construed as limiting the invention.
Embodiment 1
The preparation method of modified wood chips adsorbent is as follows:
(1) the discarded camphorwood dust of processing factory that woods, get the camphorwood dust of 500g and put into large beaker, add deionized water to wash and filter, 3 times repeatedly, until filtrate becomes limpid without muddy thing, after Separation of Solid and Liquid, obtain wet camphorwood dust, be placed in drying box, be dried 24 hours to constant weight, obtain dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve camphorwood dust particle diameter is remained between 45～75mm, make camphorwood dust powder.Get camphorwood dust powder 10g, be added in the oxalic acid solution of 200mL1.1mol/L, room temperature concussion 3 hours, shake speed is 200rpm.
(2) reaction finishes rear Separation of Solid and Liquid, respectively solid is put under the condition of 60 ℃ dry 24 hours.
(3) being warming up to 110 ℃ carries out esterification and continues 90min.
(4) be cooled to after room temperature, utilize 0.05mol/L sodium bicarbonate solution cyclic washing, until in filtrate without oxalic acid, detection method is to adopt 0.1mol/L plumbi nitras to detect filtrate.
(5) final drying sieving, obtains modified wood chips adsorbent.
Embodiment 2
The preparation method of modified wood chips adsorbent is as follows:
(1) the discarded camphorwood dust of processing factory that woods, get the camphorwood dust of 500g and put into large beaker, add deionized water to wash and filter, 3 times repeatedly, until filtrate becomes limpid without muddy thing, after Separation of Solid and Liquid, obtain wet camphorwood dust, be placed in drying box, be dried 24 hours to constant weight, obtain dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve camphorwood dust particle diameter is remained between 45～75mm, make camphorwood dust powder.Get camphorwood dust powder 10g, be added in the tartaric acid solution of 180mL1.2mol/L, room temperature concussion 3 hours, shake speed is 200rpm.
(2) reaction finishes rear Separation of Solid and Liquid, respectively solid is put under the condition of 60 ℃ dry 24 hours.
(3) being warming up to 120 ℃ carries out esterification and continues 120min.
(4) be cooled to after room temperature, utilize 0.05mol/L potassium bicarbonate solution cyclic washing, until in filtrate without tartaric acid, detection method is to adopt 0.1mol/L plumbi nitras to detect filtrate.
(5) final drying sieving, obtains modified wood chips adsorbent.
The preparation method of modified wood chips adsorbent is as follows:
(1) the discarded camphorwood dust of processing factory that woods, get the camphorwood dust of 500g and put into large beaker, add deionized water to wash and filter, 3 times repeatedly, until filtrate becomes limpid without muddy thing, after Separation of Solid and Liquid, obtain wet camphorwood dust, be placed in drying box, be dried 24 hours to constant weight, obtain dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve camphorwood dust particle diameter is remained between 45～75mm, make camphorwood dust powder.Get camphorwood dust powder 10g, be added in the citric acid solution of 240mL1.0mol/L, room temperature concussion 3 hours, shake speed is 200rpm.
(2) reaction finishes rear Separation of Solid and Liquid, respectively solid is put under the condition of 60 ℃ dry 24 hours.
(3) being warming up to 115 ℃ carries out esterification and continues 100min.
(4) be cooled to after room temperature, utilize 0.05mol/L potassium bicarbonate solution cyclic washing, until in filtrate without citric acid, detection method is to adopt 0.1mol/L plumbi nitras to detect filtrate.
(5) final drying sieving, obtains modified wood chips adsorbent.
The modification camphorwood dust that embodiment 1-3 makes contrasts figure as shown in Figure 1 with the ESEM of unmodified camphorwood dust.Unmodified camphorwood dust (a) has coarse, regular pattern composite tunnel structure, and in this structure, has random pore structure.And the camphorwood dust of modification (b), (c), (d), tunnel structure is destroyed in certain degree, but there is not too large change in fine pore structure.As shown in Figure 2, known by infrared spectrum characterization, at wavelength, be 3618.7cm
-1for the stretching vibration of O – H key causes; Wavelength 1735cm
-1and 1647.7cm
-1it is the feature of C=O key stretching vibration.Contrast unmodified wood chip, the variation at the main peak of wood chip after modification occurs in 1735cm
-1, it is sharper, higher that this peak becomes.This may be due to after organic acid modification, and a large amount of carboxyls appear at the surface of material.Above-mentioned feature shows, a large amount of active function groups (hydroxyl and carboxyl) are not only contained on sorbent material surface, also have pore structure, for the absorption of dyestuff provides a large amount of adsorption sites and larger specific area.
Embodiment 4
The application in processing waste water neutral and alkali dyestuff of modified wood chips adsorbent, step is, the modified wood chips adsorbent of embodiment 1 preparation is joined in the waste water that contains malachite green dyestuff, and addition is 0.2g/L, adopt concussion mode to mix, pH value is 8, and temperature is 35 ℃, and rotating speed is 170rpm, time is 24 hours, react complete, complete after absorption, carry out solid-liquid separation modified wood chips adsorbent.
The application in processing waste water neutral and alkali dyestuff of modified wood chips adsorbent, step is, the modified wood chips adsorbent of embodiment 2 preparations is joined in the waste water that contains methylene blue, and addition is 10g/L, employing mechanical agitation mixes, pH value is 10, and temperature is 40 ℃, and rotating speed is 170rpm, time is 10 hours, react complete, complete after absorption, carry out solid-liquid separation modified wood chips adsorbent.
The present invention can remove the basic-dyeable fibre in waste water with less adsorbent consumption.Clearance to malachite green dyestuff under the adsorbent condition of different amounts contrasts, and specifically comprises the following steps:
(1) by the adsorbent of the adsorbent of the adsorbent of oxalic acid modification, citric acid-modified and tartaric acid modification, be added into respectively in the waste water that 5 groups of malachite green dyestuff initial concentrations are 215mg/L, the volume of every group of waste water is 50mL; The consumption of described biological adsorption agent is respectively 0.2g/L, 0.6g/L, 1.0g/L, 1.4g/L, 1.8g/L.
(2) the above-mentioned waste water of respectively organizing is carried out to oscillating reactions, each oscillating reactions pH value of organizing waste water is 8.0, and oscillating reactions temperature is 35 ℃, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) waste water of respectively organizing after above-mentioned oscillating reactions is carried out to Separation of Solid and Liquid, isolate the biological adsorption agent that load has malachite green dyestuff, complete the removal to waste water Malachite Green dyestuff.
Measure the residual volume of respectively organizing wastewater sample Malachite Green dyestuff, result as shown in Figure 3.As seen from Figure 3, along with the increase of biological adsorption agent consumption, the clearance of malachite green dyestuff also increases.The wood chip of oxalic acid of the present invention, citric acid, tartaric acid modification, when the consumption of adsorbent is 1.8g/L, the clearance of malachite green dyestuff reaches respectively 99.99%, 99.91% and 97.98%.
Adsorbent of the present invention is in processing the application of waste water neutral and alkali dyestuff, and the scope of pH value is comparatively wide in range, and the present invention contrasts the clearance of malachite green dyestuff under the condition of different solutions pH, specifically comprises the following steps:
(1) by the adsorbent of the adsorbent of the adsorbent of oxalic acid modification, citric acid-modified and tartaric acid modification, be added into respectively in the waste water that 5 groups of malachite green dyestuff initial concentrations are 200mg/L, the volume of every group of waste water is 50mL; The consumption of described biological adsorption agent is respectively 1.0g/L.
(2) the above-mentioned waste water of respectively organizing is carried out to oscillating reactions, each oscillating reactions pH value of organizing waste water is respectively 3.6,4.7,5.6,6.4,8.0,9.3, and oscillating reactions temperature is 35 ℃, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) waste water of respectively organizing after above-mentioned oscillating reactions is carried out to Separation of Solid and Liquid, isolate the biological adsorption agent that load has malachite green dyestuff, complete the removal to waste water Malachite Green dyestuff.
Measure the residual volume of respectively organizing wastewater sample Malachite Green dyestuff, result as shown in Figure 4.As seen from Figure 4, along with the increase of reaction solution pH, the clearance of malachite green dyestuff also increases.The wood chip adsorbent of oxalic acid of the present invention, citric acid, tartaric acid modification, when reaction solution pH is 8.0, the clearance of malachite green dyestuff can reach respectively 98.9%, 94.4% and 76.3%.Embodiment 8
Maximum adsorption capacity of the present invention can reach 280.3mg/g, represents that 1g modification camphorwood dust adsorbent can adsorb 280.3mg basic-dyeable fibre.Adsorbent of the present invention contrasts the adsorbance of the malachite green dyestuff of different initial concentrations, specifically comprises the following steps:
(1) modification camphorwood dust adsorbent is added into respectively to 5 groups of malachite green dyestuff initial concentrations and is respectively 104mg/L, 230mg/L, 312mg/L, 424mg/L, in the waste water of 540mg/L, the volume of every group of waste water is 50mL; The consumption of described modification camphorwood dust adsorbent is 1.0g/L.
(2) the above-mentioned waste water of respectively organizing is carried out to oscillating reactions, each oscillating reactions pH value of organizing waste water is 8.0, and oscillating reactions temperature is 35 ℃, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) waste water of respectively organizing after above-mentioned oscillating reactions is carried out to Separation of Solid and Liquid, isolate the modification camphorwood dust adsorbent that load has malachite green dyestuff, complete the removal to waste water Malachite Green dyestuff.
Measure the residual volume of respectively organizing wastewater sample Malachite Green dyestuff, result as shown in Figure 5.As seen from Figure 5, the adsorbance of the modification camphorwood dust adsorbent of Unit Weight to malachite green dyestuff, increases with the concentration of initial malachite green dyestuff.The maximum adsorption capacity that can be calculated the camphorwood dust of oxalic acid, citric acid and tartaric acid modification according to Langmuir adsorption isotherm line model is respectively 280.3mg/g, 222.8mg/g and 157.5mg/g.
Below be only the preferred embodiment of the present invention, protection scope of the present invention is also not only confined to above-described embodiment, and all technical schemes belonging under thinking of the present invention all belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, some improvements and modifications without departing from the principles of the present invention, should be considered as protection scope of the present invention.
Claims (10)
1. a modified wood chips adsorbent, take wood chip as raw material, it is characterized in that, preparation method is, described wood chip and organic acid reaction, after dry, carry out esterification, remove organic acid, dry, obtain modified wood chips adsorbent, described organic acid is one or more in oxalic acid, citric acid or tartaric acid.
2. a preparation method for modified wood chips adsorbent, is characterized in that, take wood chip as raw material, described wood chip and organic acid reaction, after dry, carry out esterification, remove organic acid, dry, obtain modified wood chips adsorbent, described organic acid is one or more in oxalic acid, citric acid or tartaric acid.
3. the preparation method of modified wood chips adsorbent as claimed in claim 2, is characterized in that, comprise the steps,
(1) after wood chip is cleaned, dries, pulverized, be added in organic acid soln, mix, described organic acid soln is one or more in oxalic acid, citric acid or tartaric acid solution;
(2) mix and finish rear Separation of Solid and Liquid, wood chip solid is dried;
(3) wood chip solid is carried out to esterification under 110-120 ℃ of condition;
(4) utilize weakly alkaline solution to clean wood chip solid, until in filtrate without organic acid;
(5), to wood chip solid drying, obtain modified wood chips adsorbent.
4. the preparation method of modified wood chips adsorbent as claimed in claim 2 or claim 3, is characterized in that, described wood chip is camphorwood dust.
5. the preparation method of modified wood chips adsorbent as claimed in claim 2 or claim 3, is characterized in that, organic acid concentration is 1.0～1.2mol/L, and the mass volume ratio of wood chip and organic acid soln is 40～60g/L.
6. the preparation method of modified wood chips adsorbent as claimed in claim 3, is characterized in that, the weakly alkaline solution of step (4) is sodium acid carbonate or potassium bicarbonate solution.
7. the preparation method of modified wood chips adsorbent as claimed in claim 2 or claim 3, is characterized in that, the particle diameter of modified wood chips adsorbent is 45～75mm.
8. the modified wood chips adsorbent that the preparation method of modified wood chips adsorbent as claimed in claim 1 or claim 3 obtains is being processed containing the application in the waste water of basic-dyeable fibre.
9. application as claimed in claim 8, is characterized in that, described basic-dyeable fibre is malachite green dyestuff or methylene blue dye.
10. application as claimed in claim 8, is characterized in that, step is, described modified wood chips adsorbent is joined in the waste water that contains basic-dyeable fibre, and addition is 0.2-10g/L, mixes, and carries out after completion of the reaction Separation of Solid and Liquid, isolates the adsorbent of load basic-dyeable fibre.
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| CN104826609A (en) * | 2015-05-19 | 2015-08-12 | 湖南大学 | Method for removing hexavalent chromium in waste water by utilizing gel beads prepared from tartaric acid modified oyster mushrooms |
| CN105561938A (en) * | 2016-01-15 | 2016-05-11 | 南阳理工学院 | Method for filling static bed with saw dust to adsorb azo dye |
| CN106146758A (en) * | 2016-07-08 | 2016-11-23 | 中国地质大学（武汉） | A kind of ultraviolet light causes the method that sawdust surface grafting functional polymer prepares cation adsorbing material |
| US10913050B1 (en) | 2020-01-08 | 2021-02-09 | Prince Mohammad Bin Fahd University | Method for making and using a dye sorbent |
| CN115739037A (en) * | 2022-12-29 | 2023-03-07 | 中国科学院过程工程研究所 | High-efficiency removal of Fe in ionic liquid aqueous solution 3+ Modified wood-based adsorbent and preparation method and application thereof |
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| CN104826609A (en) * | 2015-05-19 | 2015-08-12 | 湖南大学 | Method for removing hexavalent chromium in waste water by utilizing gel beads prepared from tartaric acid modified oyster mushrooms |
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| US10913050B1 (en) | 2020-01-08 | 2021-02-09 | Prince Mohammad Bin Fahd University | Method for making and using a dye sorbent |
| US11660583B2 (en) | 2020-01-08 | 2023-05-30 | Prince Mohammad Bin Fahd University | Treatment method for forming a dye sorbent |
| CN116120114A (en) * | 2022-12-09 | 2023-05-16 | 杭州楠大环保科技有限公司 | Method for producing novel fertilizer by recycling kitchen garbage |
| CN116120114B (en) * | 2022-12-09 | 2024-01-12 | 杭州楠大环保科技有限公司 | Method for producing novel fertilizer by recycling kitchen garbage |
| CN115739037A (en) * | 2022-12-29 | 2023-03-07 | 中国科学院过程工程研究所 | High-efficiency removal of Fe in ionic liquid aqueous solution 3+ Modified wood-based adsorbent and preparation method and application thereof |
| CN115739037B (en) * | 2022-12-29 | 2024-01-26 | 中国科学院过程工程研究所 | High-efficiency Fe removal method for ionic liquid aqueous solution 3+ Modified wood-based adsorbent as well as preparation method and application thereof |
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