CN102151544A - Organic wastewater modified bentonite adsorbent and preparation method thereof - Google Patents
Organic wastewater modified bentonite adsorbent and preparation method thereof Download PDFInfo
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- CN102151544A CN102151544A CN2011100383857A CN201110038385A CN102151544A CN 102151544 A CN102151544 A CN 102151544A CN 2011100383857 A CN2011100383857 A CN 2011100383857A CN 201110038385 A CN201110038385 A CN 201110038385A CN 102151544 A CN102151544 A CN 102151544A
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Abstract
The invention discloses an organic wastewater modified bentonite absorbent and a preparation method of the absorbent. The preparation method comprises the following steps: taking organic amine type of pollutants in organic wastewater as modifying agents, taking purified bentonite powder as raw materials, adding the purified bentonite powder into the organic amine type of wastewater to agitate for 10-120 minutes at the normal temperature, and then filtering to obtain an organic wastewater modified bentonite filter cake; drying and grinding the organic wastewater modified bentonite filter cake under the condition of 90-105 DEG C to obtain organic wastewater modified bentonite, then placing the organic wastewater modified bentonite into a muffle furnace for roasting, and cooling to the normal temperature to obtain the organic wastewater modified bentonite adsorbent. The organic wastewater modified bentonite adsorbent and the preparation method have the advantages that firstly, the pollutants in the wastewater are taken as the modifying agents to realize the effect of treating the wastes with the wastes; secondly, the modification time is short; thirdly, the pollutant removal efficiency is high, and the decoloring effect is remarkable; fourthly, the solid-liquid separation is quick; and fifthly, the processing cost is low.
Description
Technical field
The present invention relates to organic wastewater modified alta-mud adsorbent and preparation method thereof.
Background technology
Bentonite is moisture lamellar aluminosilicate, and belonging to crystalline form is the hydrous alumino silicates mineral of 2: 1 three-deckers.Each crystal layer is made of folder layer of aluminum oxygen octahedra in the two-layer silicon-oxy tetrahedron, and oxygen direction structure layer central authorities in tetrahedral top are shared with octahedron, and three layers are bound up.This structure prolongs along a, b are axially unlimited, and is overlapping with certain spacing along the c direction of principal axis.The spontaneous stacked accumulation of a plurality of such wafers has formed bentonite clay particle.Chip layer is connected by weak Van der Waals force bonding or electrostatic interaction, and each interlayer dissociates easily, slides mutually sometimes.
Bentonite possesses the characteristics of hydrophilic oleophobic, its laminate interlamellar spacing is about 1.2nm, in bentonite lamella, the part high-valence cationic is by the low price cation replacement, and high isomorphous substitution between cation at a low price causes bentonite lamella negative electrical charge surplus, and superfluous negative electrical charge need be by the free NH of interlayer absorption
4 +, Na
+, Ca
2+, Mg
2+, Cu
2+, Cr
3+Come balance Deng cation, to keep its electroneutral.Therefore, bentonite can be widely used in the processing of organic amine waste water and heavy metal wastewater thereby.But owing to reasons such as the hydrophilic oleophobic of bentonite and laminate interlamellar spacing are less, be unfavorable for that octanol water partition coefficient pollutant big and the space structure complexity is approaching or enter the laminate interlayer, make that bentonitic adsorption treatment is limited in one's ability.
Modified alta-mud can overcome the above problems.Present organic modified bentonite generally adopts intercalation modifyings such as organic quaternary ammonium salt and microwave and modified synergic such as ultrasonic and gets, bentonite through organic decoration increases its lamella interlamellar spacing and specific area, improve its microscopic appearance and increase effective adsorption site position, improved being insoluble in the absorption of complicated material of water, larger molecular weight, structure by modes such as cation exchange and top layer intermolecular forces.In actual waste water was handled, organic modified bentonite then showed than better decolorizing effect of common bentonite and higher COD clearance.But, owing in processing and preparing organic modified bentonite process, used a large amount of organic quaternary ammonium salt class surfactants and rinse water and microwave and modified synergic such as ultrasonic, wastewater flow rate and pollutant have increased, and production cost and investment simultaneously all improved, and applies being affected.
Summary of the invention
The purpose of this invention is to provide a kind of organic wastewater modified alta-mud adsorbent and preparation method, the present invention can be widely used in the absorption of complicated organic amine material of larger molecular weight in the organic wastewater, structure.
Organic wastewater modified alta-mud adsorbent of the present invention is characterized in that this adsorbent is to utilize organic amine in the organic amine waste water as modifier, and the sodium base of having purified or calcium-base bentonite are carried out modification and the adsorbent that obtains.
The present invention is to be modifier with organic amine pollutant in the organic wastewater, bentonite powder with purification is a raw material, joined in the organic amine waste water stirring at normal temperature 10-120 minute, filter then, obtain organic wastewater modified alta-mud filter cake, oven dry under 90-105 ℃ of condition, grinding get the organic wastewater modified alta-mud, then it is inserted roasting in the Muffle furnace, promptly obtain organic wastewater modified alta-mud adsorbent after being cooled to normal temperature.
Purification bentonite of the present invention is to adopt sodium base or calcium-base bentonite and distilled water to mix by 1: 10 mass ratio, water-bath maintains the temperature at 40-80 ℃ and stirred 24 hours, left standstill then 6 hours, discard the sandy soil of lower floor, get supernatant liquid filtering and get filter cake, filtrate can be used for purifying next time, with filter cake 90-105 ℃ of oven dry down in baking oven, grind, cross 200 mesh sieves and make the purification bentonite.
Organic amine waste water of the present invention is meant and contains ancymidol waste water and contain benzofuranol waste water that organic amine concentration is 500mg/L-5000mg/L.
The bentonitic inventory of purification of the present invention is that the quality with organic amine pollutant in the organic amine waste water is a benchmark, with the mass ratio of organic amine pollutant be 1: 5-1: 10.
Method of roasting of the present invention is that the organic wastewater modified alta-mud was placed the Muffle furnace roasting 2-6 hour, and Muffle furnace is heated to 250-400 ℃ with the programming rate of 10-40 ℃/min, promptly gets organic wastewater modified alta-mud adsorbent of the present invention.
The present invention adopts organic amine material intercalation modification simple in structure in the organic wastewater, again with its roasting at a certain temperature, and the preparation organic modified bentonite.Organic modified bentonite through calcination process has not only improved bentonitic laminate interlamellar spacing, and organic matter part charing in roasting process, its adsorption capacity and decolorizing effect have been improved, thereby improved the adsorption treatment ability of bentonite to the organic amine pollutant of space structure complexity, reached waste water decoloring, effectively reduced the purpose of COD.
The present invention is owing to adopt 250-400 ℃ low-temperature bake, makes the organic molecule that is adsorbed on the bentonite top layer can carbonization, and the part molecule is in gasification or generate CO
2In the process that discharges, the bentonite specific area is increased to the bentonite surface etch.And the organic molecule of nexine absorption is under the obstruct of bentonite laminate, since the oxygen molecule rareness, and temperature is not high, makes it keep original molecular structure, and then increased bentonitic interlamellar spacing, improved the adsorption capacity of bentonite to the organic amine pollutant of space structure complexity.Modified alta-mud after the calcination process can be used to handle other waste water, calcination process again after intercalation, the adsorption treatment, capable of circulation applying mechanically.The present invention can obtain the adsorbent product of high-quality, can realize that again technology is simple, and is with low cost, energy-saving and emission-reduction.
The present invention compares with known technology, significantly characteristics are that pollutant in utilizing organic wastewater is as modifier, by absorption and low-temperature bake, chemisorbed and physisorption have all been strengthened to the pollutant of space structure complexity at bentonite top layer and interlayer.
The superiority that the present invention produces can fully be confirmed by Fig. 1.
Description of drawings
Fig. 1 is the XRD spectra of sodium base purification bentonite and preparation organic wastewater modified alta-mud.
The powder sample of the organic wastewater modified alta-mud of unmodified refining sodium-base bentonite and preparation is carried out XRD analysis, and abscissa is x-ray diffraction angle 2 θ among Fig. 1, and ordinate is the diffracted intensity of X ray.As can be seen from the figure 001 diffraction maximum has obvious variation.Sodium bentonite sign peak position is in 2 θ=7.4 °, and interlamellar spacing is 1.2nm; The organobentonite sign peak position of preparation is in 2 θ=4.7 °, and interlamellar spacing is 1.8nm, and this illustrates that bentonitic interlamellar spacing is effectively increased.
The specific embodiment
Used organic amine wastewater source is in Hunan insecticide factory workshop among the present invention, and the present invention is further illustrated below in conjunction with example.
Example 1: the 50g sodium bentonite is added in the 500mL distilled water, 60 ℃ of constant temperature water baths, continue to stir 24h, leave standstill 6h then, discard the sandy soil of bottom, get the supernatant suction filtration, filtrate can be used for purifying next time, filter cake is 90 ℃ of down oven dry in baking oven, and it is standby to grind the bentonite that 200 mesh sieves obtain making with extra care.
Getting ancymidol waste water 2L (ancymidol concentration is about 5000mg/L), is the sulfuric acid adjusting pH to 2 of 2mol/L with concentration.Add the refining bentonite powder of 2g, behind the stirring at normal temperature reaction 1h, suction filtration places baking oven to toast 5h down at 90 ℃, grind, place Muffle furnace to be heated to 350 ℃, roasting 4h then with the programming rate of 40 ℃/min, obtain the product of grey black look after the cooling, output is 2.17g, production code member MMT-1.
Example 2: the bentonite that obtains purifying according to the process in the example 1.
Getting benzofuranol waste water 10L (benzofuranol concentration is about 5000mg/L), is the sulfuric acid coarse adjustment pH of 10mol/L with concentration earlier, is the sulfuric acid adjusting pH to 3 of 2mol/L then with concentration.Add the refining bentonite powder of 1g, under the normal temperature behind the stirring reaction 2h, suction filtration, place baking oven to toast 5h down, grind, place Muffle furnace to be heated to 280 ℃ then with the programming rate of 40 ℃/min at 100 ℃, roasting 2h, obtain the product of grey black look after the cooling, output is 1.02g, production code member MMT-2.
Example 3: organic wastewater modified alta-mud of the present invention is tested the absorption roasting recycled of ancymidol waste water: getting above-mentioned example 1 resulting organic wastewater modified alta-mud is adsorbent, by following waste water treatment process.
1, get ancymidol waste water 100mL, the ancymidol initial concentration is 5000mg/L, and COD is 27000mg/L, and colourity is 100 times;
2, regulate pH to 3.0-5.0;
3, add organobentonite in waste water, the adsorbent consumption is the 0.5g/100mL water sample;
4, normal temperature stirs 15min down;
5, leave standstill 15min, get supernatant and with liquid chromatography residue ancymidol concentration is measured, the result shows that residual ancymidol concentration is 500mg/L, and clearance reaches 90%; Adopting the potassium bichromate Microwave Digestion to analyze rest COD is 12000mg/L; Adopt dilution method that colourity is measured, the result shows that colourity reduces to 10 times.
6, the bentonite after the absorption can also be according to the oven dry of the method for example 1, roasting, repeat 15 times after, eliminating rate of absorption still can reach 85%.
Example 4-5: implementation method is identical with example 3, and changing the waste water of handling is di-n-butylamine and tri-n-butylamine waste water.The basic condition of waste water is as shown in table 1, and adsorption conditions and result are as shown in table 2; The result is as shown in table 3 for organic wastewater modified alta-mud adsorbent replica test.Bentonite after the absorption can also repeat still have eliminating rate of absorption preferably more than 10 times according to method oven dry, the roasting of example 1.
Table 1 waste water quality basic condition
| Organic wastewater | pH | COD | Colourity |
| Di-n-butylamine waste water | 9 | 70000 | 400 |
| Tri-n-butylamine waste water | 8.7 | 30000 | 100 |
The adsorption conditions and the treatment effect of the different organic amine waste water of table 2
Table 3 organic wastewater modified alta-mud adsorbent replica test result
Claims (5)
1. organic wastewater modified alta-mud adsorbent is characterized in that this adsorbent is to utilize organic amine in the organic amine waste water as modifier, and the sodium base of having purified or calcium-base bentonite are carried out modification and the adsorbent that obtains.
2. organic wastewater modified alta-mud preparation of adsorbent method as claimed in claim 1, it is characterized in that: the bentonite powder of purifying was joined in the organic amine waste water stirring at normal temperature 10-120 minute, filter then, obtain organic wastewater modified alta-mud filter cake, oven dry under 90-105 ℃ of condition, grinding, the organic wastewater modified alta-mud, then it is inserted roasting in the Muffle furnace, promptly obtain organic wastewater modified alta-mud adsorbent after being cooled to normal temperature.
3. organic wastewater modified alta-mud preparation of adsorbent method according to claim 2, it is characterized in that described purification bentonite is to adopt sodium base or calcium-base bentonite and distilled water to mix by 1: 10 mass ratio, water-bath maintains the temperature at 40-80 ℃ and stirred 24 hours, left standstill then 6 hours, and discarded the sandy soil of lower floor, get supernatant liquid filtering and get filter cake, filtrate is used for purifying next time, with filter cake 90-105 ℃ of oven dry down in baking oven, grind, cross 200 mesh sieves and make the purification bentonite.
4. organic wastewater modified alta-mud preparation of adsorbent method according to claim 2, it is characterized in that described organic amine waste water is meant contains ancymidol waste water and contains benzofuranol waste water, organic amine concentration is 500mg/L-5000mg/L, the bentonitic inventory of described purification is that the quality with organic amine pollutant in the organic amine waste water is a benchmark, with the mass ratio of organic amine pollutant be 1: 5-1: 50.
5. organic wastewater modified alta-mud preparation of adsorbent method according to claim 2, it is characterized in that described method of roasting is that the organic wastewater modified alta-mud was placed the Muffle furnace roasting 2-6 hour, Muffle furnace is heated to 250-400 ℃ with the programming rate of 10-40 ℃/min, promptly gets organic wastewater modified alta-mud adsorbent of the present invention.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583630A (en) * | 2012-03-01 | 2012-07-18 | 山西大同大学 | Method for treating antimony-containing waste water by modified bentonite |
| CN102872809A (en) * | 2012-09-20 | 2013-01-16 | 常州大学 | Organic hydrotalcite and preparation method thereof |
| CN103496870A (en) * | 2013-09-18 | 2014-01-08 | 尹无忌 | Bentonite modifier and application thereof |
| WO2015032131A1 (en) * | 2013-09-06 | 2015-03-12 | Yin Wuji | Bentonite modifier, and modified bentonite and application thereof |
| CN107282000A (en) * | 2017-07-20 | 2017-10-24 | 安徽国能亿盛环保科技有限公司 | A kind of preparation method of modified silver type bentonite organic wastewater adsorbent |
| CN107490526A (en) * | 2017-09-06 | 2017-12-19 | 中国工程物理研究院核物理与化学研究所 | Macromolecule material aging effect the cannot-harm-detection device and its detection method |
| CN107892455A (en) * | 2017-12-18 | 2018-04-10 | 吕芳芳 | A kind of sludge treating agent for handling Organic Pollution and its preparation method and application |
| CN108059314A (en) * | 2017-12-18 | 2018-05-22 | 吕芳芳 | A kind of sludge treating agent based on vermiculite and its preparation method and application |
| CN108083589A (en) * | 2017-12-18 | 2018-05-29 | 吕芳芳 | A kind of sludge treating agent based on montmorillonite and its preparation method and application |
| CN113000017A (en) * | 2021-03-22 | 2021-06-22 | 上海果瑞环境工程有限公司 | Preparation method of modified bentonite material for treating phenol sewage |
| CN116854180A (en) * | 2023-09-04 | 2023-10-10 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583630A (en) * | 2012-03-01 | 2012-07-18 | 山西大同大学 | Method for treating antimony-containing waste water by modified bentonite |
| CN102872809A (en) * | 2012-09-20 | 2013-01-16 | 常州大学 | Organic hydrotalcite and preparation method thereof |
| WO2015032131A1 (en) * | 2013-09-06 | 2015-03-12 | Yin Wuji | Bentonite modifier, and modified bentonite and application thereof |
| US9944557B2 (en) | 2013-09-06 | 2018-04-17 | Wuji Yin | Bentonite modifier, modified bentonite, and use thereof |
| CN103496870A (en) * | 2013-09-18 | 2014-01-08 | 尹无忌 | Bentonite modifier and application thereof |
| CN107282000A (en) * | 2017-07-20 | 2017-10-24 | 安徽国能亿盛环保科技有限公司 | A kind of preparation method of modified silver type bentonite organic wastewater adsorbent |
| CN107490526B (en) * | 2017-09-06 | 2023-08-22 | 中国工程物理研究院核物理与化学研究所 | Nondestructive testing device and method for aging effect of high polymer material |
| CN107490526A (en) * | 2017-09-06 | 2017-12-19 | 中国工程物理研究院核物理与化学研究所 | Macromolecule material aging effect the cannot-harm-detection device and its detection method |
| CN107892455A (en) * | 2017-12-18 | 2018-04-10 | 吕芳芳 | A kind of sludge treating agent for handling Organic Pollution and its preparation method and application |
| CN108083589A (en) * | 2017-12-18 | 2018-05-29 | 吕芳芳 | A kind of sludge treating agent based on montmorillonite and its preparation method and application |
| CN108059314A (en) * | 2017-12-18 | 2018-05-22 | 吕芳芳 | A kind of sludge treating agent based on vermiculite and its preparation method and application |
| CN113000017A (en) * | 2021-03-22 | 2021-06-22 | 上海果瑞环境工程有限公司 | Preparation method of modified bentonite material for treating phenol sewage |
| CN116854180A (en) * | 2023-09-04 | 2023-10-10 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
| CN116854180B (en) * | 2023-09-04 | 2023-12-15 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
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Application publication date: 20110817 |