CN103566905B - Modified wood chips adsorbent, preparation method and in process containing the application in basic-dyeable fibre waste water - Google Patents
Modified wood chips adsorbent, preparation method and in process containing the application in basic-dyeable fibre waste water Download PDFInfo
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Abstract
The invention discloses a kind of modified wood chips adsorbent, preparation method and contain the application in basic-dyeable fibre waste water in process, the preparation method of modified wood chips adsorbent is, wood chip and organic acid reaction, after drying, carry out esterification, removing organic acid, dry, obtain modified wood chips adsorbent, described organic acid is one or more in oxalic acid, citric acid or tartaric acid, modified wood chips adsorbent of the present invention has the large and clearance high of simple and easy to get, adsorbance, can be applicable to the process of waste water particularly basic-dyeable fibre waste water; The cheaper starting materials adopted is easy to get, and preparation technology is simple and pollution-free, and cost is low, is easy to industrialization, achieves the object of changing waste into resources.
Description
Technical field
The present invention relates to water pollutions 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, 15% of whole world gross contamination emission is accounted for without dealing carefully with regard to the dyestuff be discharged in environment.This waste water has that color and luster is dark, stink is large, COD content is high, complicated component and changeable feature, once enter water body environment by all means, will directly or indirectly destroy ecological environment and cause serious harm to health.Therefore, how effectively to solve the problem of environmental pollution that waste water from dyestuff causes, become focus and the difficult point of people's concern.The method of current process 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 due to equipment investment few, technique and simple to operate, efficient, is with a wide range of applications.For the feature that kind of dyes in dyeing waste water is various, the key improving absorption method is to find more efficient, environmental protection, inexpensive sorbing material.
In recent years, biological material cheap and easy to get in a large number obtains more research as adsorbent in the process of waste water from dyestuff.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 NaOH aqueous solution process drying, mix with citric acid solution, cool after reaction a period of time, be washed with water to and exist without citric acid, mix with magnesium chloride solution 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, need to use NaOH solution to do basification before by citric acid treatment, need to use magnesium chloride process after by citric acid treatment, complicated process steps, the time is long, with high costs, limits it and promotes the use of.
Patent CN102266756A discloses a kind of preparation method and application thereof of citric acid modified rape straw adsorbent, grinding rape stalk, clean, after drying, need first to clean with isopropyl alcohol, mixing with sodium hydroxide solution, cleaning-drying, finally use citric acid solution process again, dry after basification, be used for removing the positive dyestuff in waste water and heavy metal ion, 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, employs 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, its maximum adsorption capacity is 125mg/g, (Gong Xinhuai etc., the dynamics of citric acid-modified bamboo bits absorption methylene blue and thermodynamic analysis, 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 adsorption capacity is low, manufacturing cost is high, raw material sources are limited etc., and shortcoming limits widely using 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 in process 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 drying, carry out esterification, removing organic acid, drying, obtains modified wood chips adsorbent, and 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, mix under room temperature, 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, stirring terminates rear Separation of Solid and Liquid, and wood chip solid is carried out drying, and baking temperature is preferably 50-70 DEG C, and the time is 24 hours.
3, be warming up to 110 ~ 120 DEG C, carry out esterification, continue 80 ~ 120min, the principle of esterification is that organic acid sticks to wood chip surface by physical action, removes moisture after drying, wood chip and organic acid generation esterification after then heating up.
4, after being cooled to 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 without organic acid in filtrate, 0.1mol/L lead nitrate solution can be adopted to detect this filtrate.
5, dry and sieve, obtain 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 in process water pollutions field, step is, the modified wood chips adsorbent above-mentioned preparation method prepared joins in the waste water containing basic-dyeable fibre, described basic-dyeable fibre is preferably malachite green dyestuff or methylene blue dye, addition is 0.2-10g/L, mechanical agitation or concussion mode is adopted to mix, the preferred rotating speed of concussion mode is 170rpm, temperature is 30-40 DEG C, time is 3-24 hour, carry out Separation of Solid and Liquid after completion of the reaction, 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 material environment being had to harm, can not produce secondary pollution to environment, with low cost, is suitable for continuously large-scale batch production; (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 force with dyestuff, as ion-exchange, electrostatic attraction and hydrogen bond etc., is beneficial to the pollution in process waste water.(4) clearance of modified wood chips adsorbent of the present invention to basic-dyeable fibre is high, and capacity is large, and use amount is little.
Accompanying drawing explanation
Fig. 1 is the ESEM contrast figure of different camphorwood dust.
Wherein, (a) is camphorwood dust, and (b) is oxalic acid modification camphorwood dust, (c) is citric acid-modified camphorwood dust, and (d) is tartaric acid modification camphorwood dust.
Fig. 2 is the infrared spectrum contrast figure of different camphorwood dust.
Wherein, (a) is camphorwood dust, and (b) is oxalic acid modification camphorwood dust, (c) is citric acid-modified camphorwood dust, and (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 that the modification camphorwood dust adsorbent of different initial concentration is to the adsorbance schematic diagram of malachite green dyestuff.
Detailed description of the invention
Below by way of specific embodiment, the present invention will be described in more detail.Embodiment is only illustrate one 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) wood the discarded camphorwood dust of processing factory, the camphorwood dust getting 500g puts into large beaker, add deionized water carry out washing 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, drying 24 is little of constant weight, obtains dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve and make camphorwood dust particle diameter remain between 45 ~ 75mm, obtained camphorwood dust powder.Get camphorwood dust powder 10g, be added in the oxalic acid solution of 200mL1.1mol/L, room temperature shakes 3 hours, and shake speed is 200rpm.
(2) reaction terminates rear Separation of Solid and Liquid, to be put into by solid respectively under the condition of 60 DEG C dry 24 hours.
(3) be warming up to 110 DEG C carry out esterification and continue 90min.
(4) after being cooled to room temperature, utilize 0.05mol/L sodium bicarbonate solution cyclic washing, until without oxalic acid in filtrate, detection method adopts 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) wood the discarded camphorwood dust of processing factory, the camphorwood dust getting 500g puts into large beaker, add deionized water carry out washing 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, drying 24 is little of constant weight, obtains dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve and make camphorwood dust particle diameter remain between 45 ~ 75mm, obtained camphorwood dust powder.Get camphorwood dust powder 10g, be added in the tartaric acid solution of 180mL1.2mol/L, room temperature shakes 3 hours, and shake speed is 200rpm.
(2) reaction terminates rear Separation of Solid and Liquid, to be put into by solid respectively under the condition of 60 DEG C dry 24 hours.
(3) be warming up to 120 DEG C carry out esterification and continue 120min.
(4) after being cooled to room temperature, utilize 0.05mol/L potassium bicarbonate solution cyclic washing, until without tartaric acid in filtrate, detection method adopts 0.1mol/L plumbi nitras to detect filtrate.
(5) final drying sieving, obtains modified wood chips adsorbent.
Embodiment 3
The preparation method of modified wood chips adsorbent is as follows:
(1) wood the discarded camphorwood dust of processing factory, the camphorwood dust getting 500g puts into large beaker, add deionized water carry out washing 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, drying 24 is little of constant weight, obtains dry camphorwood dust.Utilize high speed disintegrator, dry camphorwood dust obtained above is ground into Powdered, sieve and make camphorwood dust particle diameter remain between 45 ~ 75mm, obtained camphorwood dust powder.Get camphorwood dust powder 10g, be added in the citric acid solution of 240mL1.0mol/L, room temperature shakes 3 hours, and shake speed is 200rpm.
(2) reaction terminates rear Separation of Solid and Liquid, to be put into by solid respectively under the condition of 60 DEG C dry 24 hours.
(3) be warming up to 115 DEG C carry out esterification and continue 100min.
(4) after being cooled to room temperature, utilize 0.05mol/L potassium bicarbonate solution cyclic washing, until without citric acid in filtrate, detection method adopts 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 obtains 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 there is random pore structure on this structure.And the camphorwood dust (b) of modification, (c), (d), tunnel structure is destroyed in certain degree, but fine pore structure too large change does not occur.As shown in Figure 2, known by infrared spectrum characterization, be 3618.7cm at wavelength
-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 change at the main peak of modified wood chip occurs in 1735cm
-1, it is sharper, higher that this peak becomes.This may be due to modified through organic acid, and a large amount of carboxyls appears at the surface of material.Above-mentioned feature display, sorbent material surface not only containing a large amount of active function groups (hydroxyl and carboxyl), also has pore structure, and the absorption for dyestuff provides a large amount of adsorption sites and larger specific area.
Embodiment 4
The application in process waste water neutral and alkali dyestuff of modified wood chips adsorbent, step is, modified wood chips adsorbent embodiment 1 prepared joins in the waste water containing malachite green dyestuff, and addition is 0.2g/L, concussion mode is adopted to mix, pH value is 8, and temperature is 35 DEG C, and rotating speed is 170rpm, time is 24 hours, react complete, after completing absorption, carry out solid-liquid separation modified wood chips adsorbent.
Embodiment 5
The application in process waste water neutral and alkali dyestuff of modified wood chips adsorbent, step is, modified wood chips adsorbent embodiment 2 prepared joins in the waste water containing methylene blue, and addition is 10g/L, employing mechanical agitation mixes, pH value is 10, and temperature is 40 DEG C, and rotating speed is 170rpm, time is 10 hours, react complete, after completing absorption, carry out solid-liquid separation modified wood chips adsorbent.
Embodiment 6
The present invention can remove the basic-dyeable fibre in waste water with less adsorbent amount.The clearance of malachite green dyestuff under the adsorbent condition of different amounts is contrasted, specifically comprises the following steps:
(1) by the adsorbent of the adsorbent of oxalic acid modification, the adsorbent of citric acid-modified and tartaric acid modification, being added into 5 groups of malachite green dyestuff initial concentrations is respectively in the waste water of 215mg/L, and the volume often organizing 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) carry out oscillating reactions to above-mentioned each group of waste water, the oscillating reactions pH value of each group waste water is 8.0, and oscillating reactions temperature is 35 DEG C, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) Separation of Solid and Liquid is carried out to each group of waste water after above-mentioned oscillating reactions, 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 each group of 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 99.99%, 99.91% and 97.98% respectively.
Embodiment 7
Adsorbent of the present invention is in the application of process 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 oxalic acid modification, the adsorbent of citric acid-modified and tartaric acid modification, being added into 5 groups of malachite green dyestuff initial concentrations is respectively in the waste water of 200mg/L, and the volume often organizing waste water is 50mL; The consumption of described biological adsorption agent is respectively 1.0g/L.
(2) carry out oscillating reactions to above-mentioned each group of waste water, the oscillating reactions pH value of each group waste water is respectively 3.6,4.7,5.6,6.4,8.0,9.3, and oscillating reactions temperature is 35 DEG C, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) Separation of Solid and Liquid is carried out to each group of waste water after above-mentioned oscillating reactions, 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 each group of 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 98.9%, 94.4% and 76.3% respectively.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.The adsorbance of adsorbent of the present invention to the malachite green dyestuff of different initial concentration contrasts, and specifically comprises the following steps:
(1) modification camphorwood dust adsorbent is added into respectively 5 groups of malachite green dyestuff initial concentrations and is respectively 104mg/L, in the waste water of 230mg/L, 312mg/L, 424mg/L, 540mg/L, the volume often organizing waste water is 50mL; The consumption of described modification camphorwood dust adsorbent is 1.0g/L.
(2) carry out oscillating reactions to above-mentioned each group of waste water, the oscillating reactions pH value of each group waste water is 8.0, and oscillating reactions temperature is 35 DEG C, and oscillating reactions rotating speed is 170rpm, and the oscillating reactions time is 24 hours.
(3) Separation of Solid and Liquid is carried out to each group of waste water after above-mentioned oscillating reactions, 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 each group of wastewater sample Malachite Green dyestuff, result as shown in Figure 5.As seen from Figure 5, the modification camphorwood dust adsorbent of Unit Weight is to the adsorbance of malachite green dyestuff, and the concentration with initial malachite green dyestuff increases and increases.Can be calculated oxalic acid according to Langmuir adsorption isotherm line model, the maximum adsorption capacity of camphorwood dust of citric acid and tartaric acid modification 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 be not only confined to above-described embodiment, all technical schemes belonged 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 (6)
1. 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 drying, carry out esterification, removing organic acid, drying, obtains modified wood chips adsorbent, and described organic acid is one or more in oxalic acid, citric acid or tartaric acid; Comprise the steps,
(1), after being cleaned by wood chip, dry, pulverizing, 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) mixing terminates rear Separation of Solid and Liquid, and wood chip solid is carried out drying;
(3) wood chip solid is carried out esterification under 110-120 DEG C of condition;
(4) weakly alkaline solution is utilized to clean wood chip solid, until without organic acid in filtrate;
(5) to wood chip solid drying, modified wood chips adsorbent is obtained;
Described wood chip is camphorwood dust;
Described organic acid concentration is 1.1 ~ 1.2 mol/L, and the mass volume ratio of wood chip and organic acid soln is 40 ~ 60 g/L.
2. the preparation method of modified wood chips adsorbent as claimed in claim 1, it is characterized in that, the weakly alkaline solution of step (4) is sodium acid carbonate or potassium bicarbonate solution.
3. the preparation method of modified wood chips adsorbent as claimed in claim 1 or 2, it is characterized in that, the particle diameter of modified wood chips adsorbent is 45 ~ 75 mm.
4. the modified wood chips adsorbent that preparation method obtains as claimed in claim 1 contains the application in the waste water of basic-dyeable fibre in process.
5. apply as claimed in claim 4, it is characterized in that, described basic-dyeable fibre is malachite green dyestuff or methylene blue dye.
6. apply as claimed in claim 4, it is characterized in that, step is, joins in the waste water containing basic-dyeable fibre by described modified wood chips adsorbent, and addition is 0.2-10g/L, and mixing, carries out Separation of Solid and Liquid after completion of the reaction, isolate the adsorbent of load basic-dyeable fibre.
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| CN104826609B (en) * | 2015-05-19 | 2017-05-10 | 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 |
| CN106146758B (en) * | 2016-07-08 | 2019-01-15 | 中国地质大学（武汉） | A kind of method that ultraviolet light-initiated sawdust surface grafting functional polymer prepares cation adsorbing material |
| US11471858B2 (en) | 2020-01-08 | 2022-10-18 | Prince Mohammad Bin Fahd University | Method of producing modified sawdust sorbent |
| 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 |
| 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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| CN103212378A (en) * | 2013-04-26 | 2013-07-24 | 济南大学 | Preparation method and application of citric acid modified palm tree bark adsorbing agent |
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