CN102008943B - Method for preparing organic bentonite by using anionic dye in printing and dying wastewater - Google Patents
Method for preparing organic bentonite by using anionic dye in printing and dying wastewater Download PDFInfo
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- CN102008943B CN102008943B CN2010105197874A CN201010519787A CN102008943B CN 102008943 B CN102008943 B CN 102008943B CN 2010105197874 A CN2010105197874 A CN 2010105197874A CN 201010519787 A CN201010519787 A CN 201010519787A CN 102008943 B CN102008943 B CN 102008943B
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Abstract
The invention discloses a method for preparing organic bentonite by using anionic dye in printing and dying wastewater, belonging to the technical field of environmental pollution control and new material development. The method comprises the following steps of: adding sulfuric acid or hydrochloric acid with mass percentage of 25% to 35% into the bentonite serosity with the grain diameter of 60 meshes to 100 meshes and the moisture content of 10% to 15% to prepare slurry; digesting for 5 to 6h by steam; washing until the pH value is in the range of 4 to 5; drying and crashing under 80-110 DEG C; mixing the prepared powder product and the dry ground quick lime according to the ratio of 1:0.05-0.5; dropping water the weight of which is 2 to 2.5 times of that of the mixture; reacting for 24 to 48h under 50-65 DEG C; adding the grinded product into the printing and dying wastewater which contains the anionic dye to ensure that the mass ratio of the solid to liquid is 1:1000-10000; stirring for 4 to 5h, precipitating and separating, baking and grinding to obtain the product. In the invention, the anionic dye in the printing and dying wastewater is used as a modifier; the anionic dye in the printing and dying wastewater is effectively removed while preparing the organic bentonite; and the removing rate is higher than 95%, which achieves waste recovery.
Description
Technical field
The present invention relates to environmental pollution control and new material development technique field, relate in particular to a kind of method of utilizing anionic dye in the dyeing waste water to prepare the organobentonite adsorbent.
Background technology
Synthetic dyestuffs have complicated aromatic hydrocarbon molecular structure, and are of a great variety, are difficult to biodegradation.Some dyestuff or its catabolite have strong carcinogenic, teratogenesis, mutagenic effect, thereby the water body of dye discoloration is handled to have become one of difficult problem to be solved is arranged.It is reported that commercial dyes has 10,000 kinds approximately, the total output of annual dyestuff is 600,000 tons, and China's annual production has reached 150,000 tons, and nearly 10% ~ 20% dyestuff can directly enter environment with water in the production process, and waste water from dyestuff often has characteristics such as colourity height, toxicity be big.
Usually with dye wastewater treatment using such as physics, chemistry or biological method such as coagulating sedimentation, chemical oxidation, ion-exchange, supermembrane filter, photochemical catalytic oxidation, microorganism absorption degradations; Yet; These methods are not too obvious to the removal effect of colourity in the waste water; And disposal cost is high, and the scope of handling waste water is narrower.The mineral material of cheapness is used as the dyestuff in the adsorbents adsorb waste water, and with low cost, the source is abundant.
Bentonite be a kind of be the clay rock that essential mineral is formed with the montmorillonite; Montmorillonite since in the broken key, lattice isomorph replace and to be adsorbed on its surperficial humus disassociation etc. former thereby electronegative; Thereby cause combining between lattice layer to loosen, meet water and be prone to expand into fragment, the particle decentralization is high; Have huge internal surface area and a large amount of exchangeable cations, have good adsorption performance and ion-exchange performance.Quaternary cationic surfactant can get into bentonitic interlayer through ion exchange; Significantly change the size of bentonitic two-dimensional nano sheet interlayer; Interlayer becomes hydrophobicity by hydrophily; It is main that adsorption mechanism becomes distributional effects by surface adsorption, and the efficient that organic pollution in the water is removed in absorption arrives hundred times than original soil high tens.But owing to cationic surfactant costs an arm and a leg, thereby cause the bentonite price also very expensive, seriously limited the application of organobentonite aspect water treatment.
Summary of the invention
The objective of the invention is for overcoming the deficiency of prior art, provide a kind of anionic dye that exists in the dyeing waste water that utilizes to come modified alta-mud, and be used for treatment of Organic Wastewater as adsorbent.
The technical scheme that the present invention adopts is in turn include the following steps:
1) is that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry with mass fraction, fully stirs, process mud; Use steam digestion 5 ~ 6h again; Whenever therebetween, stirred once at a distance from 15 minutes, through wash to pH be 4 ~ 5, concentrated; Filter, 80 ℃ ~ 110 ℃ dry down and pulverizing;
2) with powdery product that makes and dry quick lime powder mixed according to 1:0.05 ~ 0.5; Be added dropwise to the water of weight while stirring again, stir into pasty state, place thermostatic drying chamber for 2 ~ 2.5 times in this mixture; In temperature is 50 ~ 65 ℃ of reaction 24h ~ 48h down; Wash 4 ~ 5 times, oven dry is milled;
3) will the mill product that obtains adds and contains in the dyeing waste water of anionic dye, and the solid-liquid mass ratio is 1:1000 ~ 10000, stirs 4 ~ 5h, precipitate and separate, and oven dry, milling gets final product.
The invention has the beneficial effects as follows:
1, the present invention is a modifier with the anionic dye in the dyeing waste water, utilizes the anionic dye that exists in the dyeing waste water to synthesize organobentonite.At the preparation bentonite simultaneously, effectively the anionic dye in the dyeing waste water is removed in absorption, has not only removed the anionic dye in the waste water but also has synthesized organobentonite, realizes waste recovery.
2, prepared organobentonite is cheap, and water treatment effect is obvious, and clearance is higher than 95%, reaches the effect of the treatment of wastes with processes of wastes against one another, has very strong economy and practical value.
The specific embodiment
Be that 25% ~ 35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders ~ 100 orders and water content are 10 ~ 15% bentonite slurry with mass fraction earlier, bentonite can adopt sodium bentonite or calcium-base bentonite, through fully stirring; Process mud, use steam digestion 5 ~ 6h again, whenever stirred once therebetween at a distance from 15 minutes; Through wash to pH be 4 ~ 5; Concentrate, filter, drying is also pulverized under 80 ℃ ~ 110 ℃.Then with powdery product that makes and dry quick lime powder mixed according to 1:0.05 ~ 0.5; Be added dropwise to the water of weight while stirring again, stir into pasty state, place thermostatic drying chamber for 2 ~ 2.5 times in this mixture; In temperature is 50 ~ 65 ℃ of reaction 24h ~ 48h down; Wash 4 ~ 5 times, oven dry is milled; The product adding that obtains of will milling at last contains in the dyeing waste water of anionic dye, and the solid-liquid mass ratio is 1:1000 ~ 10000, stirs 4 ~ 5h, precipitate and separate, and oven dry, milling gets final product.
4 embodiment of the present invention below further are provided:
Embodiment 1
With mass fraction is that 25% hydrochloric acid adds particle diameter in 60 order order water content are 12% sodium bentonite slurries, fully stirs, and processes mud; Use steam digestion 5 h again, stirred once in per therebetween 15 minutes, through wash to pH be 4; Concentrate, filter, drying is also pulverized under 80 ℃; Powder that makes and the dry quick lime powder proportion according to 1:0.05 are mixed, stir again on one side and be added dropwise to the water that weight is 2 times in this mixture, stir into pasty state; Placing thermostatic drying chamber, is 50 ℃ of reaction 24h down in temperature, washes 4 times; Oven dry is milled; In the waste water that contains anionic dye gold orange II that the product that obtains milling adds, solid-to-liquid ratio is that 1:1000 stirs 4h, precipitate and separate, and oven dry, milling obtains organobentonite.
In 200 mL conical flasks, adding 50mL, to contain luxuriant and rich with fragrance concentration be 1 mg/L waste water, adds 25 mg organobentonites.Put into constant temperature oscillator, at 25 ℃, vibration is 2 hours under the 200 rpm conditions, takes out the back centrifugation, measures concentration with ultraviolet-uisible spectrophotometer, and clearance is 98.8%.
Embodiment 2
With mass fraction is that 25% hydrochloric acid adds particle diameter in 100 order water content are 10% calcium-base bentonite slurries, fully stirs, and processes mud; Use steam digestion 6h again, stirred once in per therebetween 15 minutes, through wash to pH be 5; Concentrate, filter, drying is also pulverized under 110 ℃; Powder that makes and the dry quick lime powder proportion according to 1:0.5 are mixed, stir again on one side and be added dropwise to the water that weight is 2 times in this mixture, stir into pasty state; Placing thermostatic drying chamber, is 50 ℃ of reaction 48h down in temperature, washes 5 times; Oven dry is milled; What the product that obtains milling added contains in the Congo red waste water of anionic dye, and solid-to-liquid ratio is that 1:10000 stirs 5h, precipitate and separate, and oven dry, milling obtains organobentonite.
In 200 mL conical flasks, adding 50mL, to contain beta naphthal concentration be 15 mg/L waste water, adds 25 mg organobentonites.Put into constant temperature oscillator, at 25 ℃, vibration is 2 hours under the 200 rpm conditions, takes out the back centrifugation, measures concentration with ultraviolet-uisible spectrophotometer, and clearance is 95.5%.
Embodiment 3
With mass fraction is that 35% sulfuric acid adds particle diameter in 100 order water content are 13% calcium-base bentonite slurries, fully stirs, and processes mud; Use steam digestion 6h again, stirred once in per therebetween 15 minutes, through wash to pH be 5; Concentrate, filter, drying is also pulverized under 110 ℃; Powder that makes and the dry quick lime powder proportion according to 1:0.5 are mixed, stir again on one side and be added dropwise to the water that weight is 2.5 times in this mixture, stir into pasty state; Placing thermostatic drying chamber, is 65 ℃ of reaction 24h down in temperature, washes 4 times; Oven dry is milled; In the waste water that contains anionic dye gold orange II that the product that obtains milling adds, solid-to-liquid ratio is that 1:10000 stirs 5h, precipitate and separate, and oven dry, milling obtains organobentonite.
In 200 mL conical flasks, adding 50mL, to contain phenol concentration be 30 mg/L waste water, adds 25 mg organobentonites.Put into constant temperature oscillator, at 25 ℃, vibration is 2 hours under the 200 rpm conditions, takes out the back centrifugation, measures concentration with ultraviolet-uisible spectrophotometer, and clearance is 95.1%.
Embodiment 4
With mass fraction is that 35% sulfuric acid adds particle diameter in 60 order water content are 15% sodium bentonite slurries, fully stirs, and processes mud; Use steam digestion 5h again, stirred once in per therebetween 15 minutes, through wash to pH be 5; Concentrate, filter, drying is also pulverized under 110 ℃; Powder that makes and the dry quick lime powder proportion according to 1:0.5 are mixed, stir again on one side and be added dropwise to the water that weight is 2.5 times in this mixture, stir into pasty state; Placing thermostatic drying chamber, is 65 ℃ of reaction 48h down in temperature, washes 4 times; Oven dry is milled; In the waste water that contains acid fuchsin that the product that obtains milling adds, solid-to-liquid ratio is that 1:1000 stirs 5h, precipitate and separate, and oven dry, milling obtains organobentonite.
In 200 mL conical flasks, adding 20mL nitrobenzene-containing concentration is 5 mg/L waste water, adds 25 mg organobentonites.Put into constant temperature oscillator, at 25 ℃, vibration is 2 hours under the 200 rpm conditions, takes out the back centrifugation, measures concentration with ultraviolet-uisible spectrophotometer, and clearance is 96.8%.
Claims (1)
1. one kind is utilized that anionic dye prepares the bentonite method in the dyeing waste water, it is characterized in that in turn including the following steps:
1) is that 25%～35% sulfuric acid or hydrochloric acid add particle diameter in 60 orders～100 orders and water content are 10～15% bentonite slurry with mass fraction, fully stirs, process mud; Use steam digestion 5～6h again; Whenever therebetween, stirred once at a distance from 15 minutes, through wash to pH be 4～5, concentrated; Filter, 80 ℃～110 ℃ dry down and pulverizing;
2) with the powdery product that makes and dry quick lime powder according to 1: 0.05～0.5 mixed; Be added dropwise to the water of weight while stirring again, stir into pasty state, place thermostatic drying chamber for 2～2.5 times in this mixture; In temperature is 50～65 ℃ of reaction 24h～48h down; Wash 4～5 times, oven dry is milled;
3) will the mill product that obtains adds and contains in the dyeing waste water of anionic dye, and making the solid-liquid mass ratio is 1: 1000～10000, stirs 4～5h, precipitate and separate, and oven dry, milling gets final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010105197874A CN102008943B (en) | 2010-10-26 | 2010-10-26 | Method for preparing organic bentonite by using anionic dye in printing and dying wastewater |
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| CN2010105197874A CN102008943B (en) | 2010-10-26 | 2010-10-26 | Method for preparing organic bentonite by using anionic dye in printing and dying wastewater |
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| CN102008943B true CN102008943B (en) | 2012-05-30 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102659208A (en) * | 2012-05-24 | 2012-09-12 | 苏州科技学院 | Treatment method for dye wastewater |
| CN102847513A (en) * | 2012-09-19 | 2013-01-02 | 常州大学 | Method for preparing organic hydrotalcite |
| CN102974313A (en) * | 2012-11-28 | 2013-03-20 | 常州大学 | Method for preparing organic hydrotalcite by using negative anionic dye in printing and dyeing wastewater |
| CN109174064A (en) * | 2018-10-19 | 2019-01-11 | 华北水利水电大学 | The preparation of bentonite-moringa seeds albumen composite adsorbing material and its application method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279239A (en) * | 2008-01-21 | 2008-10-08 | 浙江瑞普环境技术有限公司 | Organic modified mineral adsorbing material and method of producing the same |
| CN101757886A (en) * | 2010-02-09 | 2010-06-30 | 浙江林学院 | Production method of environment-friendly chitosan intercalation composite bentonite adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5447881A (en) * | 1977-09-22 | 1979-04-14 | Hiroya Inaba | Surfactant associating and aggregating agent |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279239A (en) * | 2008-01-21 | 2008-10-08 | 浙江瑞普环境技术有限公司 | Organic modified mineral adsorbing material and method of producing the same |
| CN101757886A (en) * | 2010-02-09 | 2010-06-30 | 浙江林学院 | Production method of environment-friendly chitosan intercalation composite bentonite adsorbent |
Non-Patent Citations (3)
| Title |
|---|
| Dazhong Shen et al..Adsorption kinetics and isotherm of anionic dyes onto organo-bentonite from single and multisolute systems.《Journal of Hazardous Materials》.2009,第172卷 * |
| JP特开昭54-47881A 1979.04.14 |
| 杨立红等.膨润土的改性及在有机废水处理中的应用.《世界地质》.2001,第20卷(第1期), * |
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